Tag: M.W=500-600

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 289042-12-2, name is tert-Butyl 2-((4R,6S)-6-((E)-2-(4-(4-fluorophenyl)-6-isopropyl-2-(N-methylmethylsulfonamido)pyrimidin-5-yl)vinyl)-2,2-dimethyl-1,3-dioxan-4-yl)acetate, the common compound, a new synthetic route is introduced below. Safety of tert-Butyl 2-((4R,6S)-6-((E)-2-(4-(4-fluorophenyl)-6-isopropyl-2-(N-methylmethylsulfonamido)pyrimidin-5-yl)vinyl)-2,2-dimethyl-1,3-dioxan-4-yl)acetate

A solution of the compound of formula (39) (7.0 g, 12.1 MMOL) and CAMPHOR-1 0-SULFONIC ACID (2.4 g, 10.4 MMOL) in acetonitrile (50 ml) and water (5 ml) is stirred at room temperature for 30 minutes. It is then diluted with ether and washed successively with saturated sodium hydrogen carbonate solution and brine. The organic phase is dried (using NA2SO4). The salt mixture is filtered off and the filtrate obtained is concentrated by evaporation. The concentrated crude product is dissolved in ethyl acetate and made to crystallise by adding hexane. In that manner, 1.6 G (57 %) of the desired product (41) can be obtained in the form of colourless crystals. ‘H NMR (300 MHz, DMSO-DE) : 1.22 (d, J = 6.7 Hz, 6H); 1.32-1. 44 (m, 1H) ; 1. 38 (s, 9H); 1.49-1. 59 (m, 1H); 2.20 (dd, J = 15.0, 7.9 Hz, 1H); 2.28 (DD, J = 15.0, 5.3 Hz, 1H); 3.39-3. 47 (m, 1H) ; 3.44 (s, 3H); 3.53 (s, 3H); 3.74-3. 85 (M, 1H) ; 4.14-4. 22 (m, 1H) ; 4.64 (d, J = 5.3 Hz, 1H) ; 4.89 (d, J = 4.7 Hz, 1H) ; 5.51 (dd, J = 16.1, 5.6 Hz, 1H) ; 6.51 (dd, J = 16. 1,1. 2 Hz, 1H) ; 7.25 (dd, J = 8.8, 8.8 Hz, 2H); 7.70 (dd, J = 9.1, 5.6 Hz, 2H). 13C NMR (75 MHz, DMSO-DB) : 22.4, 28.6, 32.1, 34.0, 42.4, 44.4, 44.9, 65.9, 69.2, 80. 2, 115.7 (JCF = 21.7 Hz), 122.1, 122.4, 132.8 (JCF = 8.7 Hz), 135.1 (JCF = 3.2 Hz), 141.9, 157.4, 163.2 (JCF = 249 Hz), 163.4, 171.1, 174.9. HPLC: CHIRALCEL OD (0.46×25 cm), hexane: EtOH 95: 5,1 ml/min, TR = 19.2 min, S 98 % ee.

The synthetic route of 289042-12-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CIBA SPECIALTY CHEMICALS HOLDING INC.; WO2004/103977; (2004); A2;,
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Reference of 274693-26-4, Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 274693-26-4, name is 2-(((3aR,4S,6R,6aS)-6-(7-(((1R,2S)-2-(3,4-Difluorophenyl)cyclopropyl)amino)-5-(propylthio)-3H-[1,2,3]triazolo[4,5-d]pyrimidin-3-yl)-2,2-dimethyltetrahydro-3aH-cyclopenta[d][1,3]dioxol-4-yl)oxy)ethanol. A new synthetic method of this compound is introduced below.

(1) cooling the toluene solution of the upper step product remaining in the 200L reaction vessel to 10 to 20 C;(2) adding 37.062 kg of hydrochloric acid and 55 L of methanol mixed solution cooled to 10 to 20 C into the reaction kettle under stirring;After the addition is completed, the mixture is kept at 10 to 20 C for 3 to 4 hours;(3) TLC detection reaction was completed, ethyl acetate: isooctane = 1:1, and the upper organic phase plate was taken;Stop stirring, let stand for stratification, and separate the lower methanol water phase for use;(4) adding a lower methanol aqueous phase separated in the above step to a 500 L reaction kettle, and adding 20% potassium carbonate aqueous solution (25.406 kg of potassium carbonate and 101.64 L of purified water) under stirring;Finally adjust the pH between 7-9;(5) adding 55 L of ethyl acetate under stirring, and stirring for 30 min;Stop stirring, let stand layering, separate the lower layer of water, and transfer the upper organic phase to the PE barrel for use;(6) The lower aqueous phase was transferred to the reaction vessel, 55 L of ethyl acetate was added, and the mixture was stirred for 30 minutes; the stirring was stopped, the layer was allowed to stand, and the lower aqueous phase was separated; (7) Combine the two organic phases, add 200L reaction kettle, add 55L purified water under stirring, and stir for 30 minutes;Stop stirring, let stand for stratification, and separate the lower aqueous phase;Then, 55 L of purified water was added to the reaction vessel, and the mixture was stirred for 30 minutes; the stirring was stopped, the layer was allowed to stand, and the lower aqueous phase was separated;(8) adding 686 g of activated carbon to the organic phase (the amount of activated carbon is 5% of the crude product, the crude product is calculated in 100% yield), heating to 40-50 C, stirring for 30 minutes;(9) Filter the filter pad with diatomaceous earth (about 100 g of diatomaceous earth), distill off the solvent under reduced pressure at 50 C, and steam until no more liquid flows out;Then add 11 L of ethyl acetate to distill off the solvent, repeat 2 times until the solid is produced, no more liquid will flow out;To the residue, 68.61 L of ethyl acetate was added and heated to 50-60 C to dissolve (the amount of ethyl acetate was 5 times the mass of the crude product, and the crude product was calculated in 100% yield);Transfer the solution to a 50L reactor and heat to 50-60 C; (10) adding 82.33 L of isooctane preheated to 50-60 C under stirring (the amount of isooctane is 1.2 times the volume of ethyl acetate);Control the addition speed to keep the internal temperature above 50 C, and gradually precipitate solids during the addition;(11) After the addition is completed, the temperature is lowered by stirring to a temperature of 20 to 30 C, and stirred for 1 hour;(12) further cooling to 0 to 10 C and stirring for 2 hours;(13) centrifugal filtration, the reaction kettle and the filter cake are washed with a mixture of 13.72 L of ethyl acetate and 16.47 L of isooctane precooled to 0 to 10 C;(14) The filter cake was dried under vacuum at 45 to 55 C for 8 to 12 hours to obtain 11.6 kg of ticagrelor crude product (Im-4); the yield was 85%. (1) Add 45 L of dichloromethane and 108 L of t-butanol to a 200 L crystallizer; add 11.5 kg of ticagrelor crude by stirring. (2) heating to 50 ~ 60 C under stirring for 1 hour; cooling to 20 ~ 30 C, stirring for 1 hour;(3) further cooling to 0 to 10 C for 2 hours;(4) centrifugal filtration, the reaction kettle and the filter cake are rinsed with water precooled to 0 to 10 C;(5) The filter cake was dried under vacuum at 45-55 C for 8 to 12 hours to obtain 10.7 kg of ticagrelor; the weight yield was 93%. After testing total impurities of 0.74%, SM1: 0.09%, Im-1: 0.08%

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,274693-26-4, its application will become more common.

Reference:
Patent; Beijing Dongxuli Pharmaceutical Technology Co., Ltd.; Bao Yiwen; Wang Yajun; (20 pag.)CN108329320; (2018); A;,
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As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 355806-00-7, name is (3R,5S,6E)-7-[4-(4-Fluorophenyl)-6-isopropyl-2-[(methanesulfonyl) methylamino]pyrimidin-5-yl]-3,5-dihydroxyhept-6-enoic acid tert-butyl ester, molecular formula is C26H36FN3O6S, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. Application In Synthesis of (3R,5S,6E)-7-[4-(4-Fluorophenyl)-6-isopropyl-2-[(methanesulfonyl) methylamino]pyrimidin-5-yl]-3,5-dihydroxyhept-6-enoic acid tert-butyl ester

Example-2:40 g of Rosuvastatin diol ester as prepared in example-1 above was taken in 400 mL of methanol at 25C to 35nC and cooled to 20″-25″C. The mixture of sodium hydroxide (3.6 g) and water (72 mL) solution was added to above solution within 30 minutes. After complete addition, the solution was stirred and further cooled to 10- 200C. The pH was adjusted between 7.5-8.5 by IN HCl (17 mL). Remaining mixture was washed with toluene at 20 to 300C. The aqueous layer was subjected to distillation under vacuum to remove MeOH below 500C till remaining volume becomes 130 mL. The volume was adjusted to 250 mL by adding water. The remaining mixture was passed through hydrobed and washed with water. A solution of 10.3 g calcium chloride in 40 mL water was added to the reaction mixture and the solution was filtered at 150C to 200C. The temperature was raised upto 250C to 35C and stirred for 1 hr. The product was filtered and washed with water. The product was dried at 500C to 55C to get 34.7 g of Rosuvastatin Calcium having individual impurity less than 0.1% HPLC Purity > 99.65% .

With the rapid development of chemical substances, we look forward to future research findings about 355806-00-7.

Reference:
Patent; CADILA HEALTHCARE LIMITED; WO2007/99561; (2007); A1;,
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Synthetic Route of 1195768-23-0, Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 1195768-23-0, name is N-(3-(2-(tert-Butyl)-5-(2-chloropyrimidin-4-yl)thiazol-4-yl)-2-fluorophenyl)-2,6-difluorobenzenesulfonamide. A new synthetic method of this compound is introduced below.

Step D : N- { 3 – [ 5-(2-amino-4-pyrimidiny l)-2-( 1 , 1 -dimethy lethyl)- 1 ,3 -thiazol-4-yl] -2- fluorophenyl} -2,6-difluorobenzenesulfonamide: In 1 gal pressure reactor, a mixture of N- {3-[5-(2-chloro-4-pyrimidinyl)-2-(l,l- dimethylethyl)-l,3-thiazol-4-yl]-2-fluorophenyl} -2,6-difluorobenzenesulfonamide (120 g) prepared in accordance with Step C, above, and ammonium hydroxide (28-30%, 2.4 L, 20 vol) was heated in the sealed pressure reactor to 98-103 C and stirred at this temperature for 2 hours. The reaction was cooled slowly to room temperature (20 C) and stirred overnight. The solids were filtered and washed with minimum amount of the mother liquor and dried under vacuum. The solids were added to a mixture of EtOAc (15 vol)/ water (2 vol) and heated to complete dissolution at 60-70 C and the aqueous layer was removed and discarded. The EtOAC layer was charged with water (1 vol) and neutralized with aq. HC1 to ~pH 5.4-5.5. and added water (lvol). The aqueous layer was removed and discarded at 60-70 C. The organic layer was washed with water (1 vol) at 60-70 C and the aqueous layer was removed and discarded. The organic layer was filtered at 60 C and concentrated to 3 volumes. EtOAc (6 vol) was charged into the mixture and heated and stirred at 72 C for 10 min , then cooled to 20C and stirred overnight. EtOAc was removed via vacuum distillation to concentrate the reaction mixture to ~3 volumes. The reaction mixture was maintained at ~65-70C for ~30mins. Product crystals having the same crystal form as those prepared in Example 58b (and preparable by the procedure of Example 58b), above, in heptanes slurry were charged. Heptane (9 vol) was slowly added at 65-70 C. The slurry was stirred at 65-70 C for 2-3 hours and then cooled slowly to 0-5C. The product was filtered, washed with EtO Ac/heptane (3/1 v/v, 4 vol) and dried at 45 C under vacuum to obtain N- {3 – [5 -(2-amino-4-pyrimidinyl)-2-( 1 , 1 -dimethylethyl)- 1 , 3 -thiazol-4-yl] -2- fluorophenyl}-2,6-difluorobenzenesulfonamide (102.3 g, 88%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,1195768-23-0, its application will become more common.

Reference:
Patent; NOVARTIS AG; CAPONIGRO, Giordano; HORN-SPIROHN, Thomas; LEHAR, Joseph; (49 pag.)WO2017/37587; (2017); A1;,
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Reference of 1195768-23-0 , The common heterocyclic compound, 1195768-23-0, name is N-(3-(2-(tert-Butyl)-5-(2-chloropyrimidin-4-yl)thiazol-4-yl)-2-fluorophenyl)-2,6-difluorobenzenesulfonamide, molecular formula is C23H18ClF3N4O2S2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.

Step D: A/-{3-[5-(2-amino-4-pyhmidinyl)-2-(1 ,1 -dimethylethyl)-1 ,3-thiazol-4-yl]-2- fluorophenyl}-2,6-difluorobenzenesulfonannideIn 1 gal pressure reactor, a mixture of A/-{3-[5-(2-chloro-4-pyrinnidinyl)-2-(1 ,1 – dimethylethyl)-1 ,3-thiazol-4-yl]-2-fluorophenyl}-2,6-difluorobenzenesulfonamide (120 g) prepared in accordance with Step C, above, and ammonium hydroxide (28-30%, 2.4 L, 20 vol) was heated in the sealed pressure reactor to 98-103 C and stirred at this temperature for 2 hours. The reaction was cooled slowly to room temperature (20 C) and stirred overnight. The solids were filtered and washed with minimum amount of the mother liquor and dried under vacuum. The solids were added to a mixture of EtOAc (15 vol)/ water (2 vol) and heated to complete dissolution at 60-70 C and the aqueous layer was removed and discarded. The EtOAC layer was charged with water (1 vol) and neutralized with aq. HCI to ~pH 5.4-5.5. and added water (1 vol). The aqueous layer was removed and discarded at 60-70 C. The organic layer was washed with water (1 vol) at 60-70 C and the aqueous layer was removed and discarded. The organic layer was filtered at 60 C and concentrated to 3 volumes. EtOAc (6 vol) was charged into the mixture and heated and stirred at 72 C for 10 min , then cooled to 20C and stirred overnight. EtOAc was removed via vacuum distillation to concentrate the reaction mixture to ~3 volumes. The reaction mixture was maintained at ~65-70C for ~30mins. Product crystals having the same crystal form as those prepared in Example 58b (and preparable by the procedure of Example 58b), above, in heptanes slurry were charged. Heptane (9 vol) was slowly added at 65-70 C. The slurry was stirred at 65-70 C for 2- 3 hours and then cooled slowly to 0-5C. The product was filtered, washed withEtOAc/heptane (3/1 v/v, 4 vol) and dried at 45C under vacuum to obtain A/-{3-[5-(2- amino-4-pyrimidinyl)-2-(1 ,1 -dimethylethyl)-1 ,3-thiazol-4-yl]-2-fluorophenyl}-2,6- difluorobenzenesulfonamide (102.3 g, 88%).

The synthetic route of 1195768-23-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXOSMITHKLINE LLC; DUMBLE, Melissa; KUMAR, Rakesh; LAQUERRE, Sylvie; LEBOWITZ, Peter; WO2011/47238; (2011); A1;,
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Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 274693-26-4, name is 2-(((3aR,4S,6R,6aS)-6-(7-(((1R,2S)-2-(3,4-Difluorophenyl)cyclopropyl)amino)-5-(propylthio)-3H-[1,2,3]triazolo[4,5-d]pyrimidin-3-yl)-2,2-dimethyltetrahydro-3aH-cyclopenta[d][1,3]dioxol-4-yl)oxy)ethanol. This compound has unique chemical properties. The synthetic route is as follows. Safety of 2-(((3aR,4S,6R,6aS)-6-(7-(((1R,2S)-2-(3,4-Difluorophenyl)cyclopropyl)amino)-5-(propylthio)-3H-[1,2,3]triazolo[4,5-d]pyrimidin-3-yl)-2,2-dimethyltetrahydro-3aH-cyclopenta[d][1,3]dioxol-4-yl)oxy)ethanol

The intermediate TG-3 obtained in the step S3 is added to the reactor, and then dissolved in methanol, and the temperature is lowered to 2 C, and nitrogen gas is added thereto, and the methanol solution of hydrochloric acid is added dropwise under the temperature control for 2 hours. Water and ethyl acetate were added, the system was temperature-controlled at 15 C, and the liquid phase was separated. The aqueous phase was extracted twice with 5 times TG-3 weight of ethyl acetate. The organic phase was washed once with saturated aqueous sodium hydrogencarbonate and the organic layer was evaporated to dryness. After adding ethyl acetate, stirring to complete dissolution, heating to reflux, adding n-hexane dropwise, stirring and cooling to 22 C, stirring was continued for 1.5 h, filtration, and vacuum drying to obtain white solid TG-4 as a crude product; The mass ratio of TG-3, methanol, methanolic hydrochloric acid solution, water, ethyl acetate and n-hexane was 1:2.5:2.5:3:2:4.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, 274693-26-4, 2-(((3aR,4S,6R,6aS)-6-(7-(((1R,2S)-2-(3,4-Difluorophenyl)cyclopropyl)amino)-5-(propylthio)-3H-[1,2,3]triazolo[4,5-d]pyrimidin-3-yl)-2,2-dimethyltetrahydro-3aH-cyclopenta[d][1,3]dioxol-4-yl)oxy)ethanol.

Reference:
Patent; Jiangxi Sinopharm Co., Ltd.; Yang Jianguo; Wan Yibin; Ge Youqun; Zuo Feihong; Yu Chengxiang; Yang Ming; Li Jinjin; Yu Lianxin; Liu Wei; Xie Liangliang; Liu Linhua; (19 pag.)CN108892670; (2018); A;,
Pyrimidine | C4H4N2 – PubChem,
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Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 355806-00-7, name is (3R,5S,6E)-7-[4-(4-Fluorophenyl)-6-isopropyl-2-[(methanesulfonyl) methylamino]pyrimidin-5-yl]-3,5-dihydroxyhept-6-enoic acid tert-butyl ester. This compound has unique chemical properties. The synthetic route is as follows. Quality Control of (3R,5S,6E)-7-[4-(4-Fluorophenyl)-6-isopropyl-2-[(methanesulfonyl) methylamino]pyrimidin-5-yl]-3,5-dihydroxyhept-6-enoic acid tert-butyl ester

Example 1; Hydrolysis of terf-butyl ester of rosuvastatin in aqueous solution of amines; 7.5 g of terf-butyl ester of rosuvastatin 38 ml of demineralized water 2 to 5 equivalents of amineThe reactants and water as the solvent are stirred in the autoclave from 98 to 1000C for 1 to 4 hours. The reaction mixture is sampled and analyzed by HPLC (“High Pressure Liquid Chromatography”) to find out the completion of reaction. Results are shown in Table 1. EPO

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, 355806-00-7, (3R,5S,6E)-7-[4-(4-Fluorophenyl)-6-isopropyl-2-[(methanesulfonyl) methylamino]pyrimidin-5-yl]-3,5-dihydroxyhept-6-enoic acid tert-butyl ester.

Reference:
Patent; LEK PHARMACEUTICALS D.D.; WO2006/136407; (2006); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 274693-26-4, name is 2-(((3aR,4S,6R,6aS)-6-(7-(((1R,2S)-2-(3,4-Difluorophenyl)cyclopropyl)amino)-5-(propylthio)-3H-[1,2,3]triazolo[4,5-d]pyrimidin-3-yl)-2,2-dimethyltetrahydro-3aH-cyclopenta[d][1,3]dioxol-4-yl)oxy)ethanol. This compound has unique chemical properties. The synthetic route is as follows. Safety of 2-(((3aR,4S,6R,6aS)-6-(7-(((1R,2S)-2-(3,4-Difluorophenyl)cyclopropyl)amino)-5-(propylthio)-3H-[1,2,3]triazolo[4,5-d]pyrimidin-3-yl)-2,2-dimethyltetrahydro-3aH-cyclopenta[d][1,3]dioxol-4-yl)oxy)ethanol

The intermediate TG-3 obtained in the step S3 is added to the reactor, and then dissolved in methanol, and the temperature is lowered to 2 C, and nitrogen gas is added thereto, and the methanol solution of hydrochloric acid is added dropwise under the temperature control for 2 hours. Water and ethyl acetate were added, the system was temperature-controlled at 15 C, and the liquid phase was separated. The aqueous phase was extracted twice with 5 times TG-3 weight of ethyl acetate. The organic phase was washed once with saturated aqueous sodium hydrogencarbonate and the organic layer was evaporated to dryness. After adding ethyl acetate, stirring to complete dissolution, heating to reflux, adding n-hexane dropwise, stirring and cooling to 22 C, stirring was continued for 1.5 h, filtration, and vacuum drying to obtain white solid TG-4 as a crude product; The mass ratio of TG-3, methanol, methanolic hydrochloric acid solution, water, ethyl acetate and n-hexane was 1:2.5:2.5:3:2:4.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, 274693-26-4, 2-(((3aR,4S,6R,6aS)-6-(7-(((1R,2S)-2-(3,4-Difluorophenyl)cyclopropyl)amino)-5-(propylthio)-3H-[1,2,3]triazolo[4,5-d]pyrimidin-3-yl)-2,2-dimethyltetrahydro-3aH-cyclopenta[d][1,3]dioxol-4-yl)oxy)ethanol.

Reference:
Patent; Jiangxi Sinopharm Co., Ltd.; Yang Jianguo; Wan Yibin; Ge Youqun; Zuo Feihong; Yu Chengxiang; Yang Ming; Li Jinjin; Yu Lianxin; Liu Wei; Xie Liangliang; Liu Linhua; (19 pag.)CN108892670; (2018); A;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 355806-00-7, name is (3R,5S,6E)-7-[4-(4-Fluorophenyl)-6-isopropyl-2-[(methanesulfonyl) methylamino]pyrimidin-5-yl]-3,5-dihydroxyhept-6-enoic acid tert-butyl ester. This compound has unique chemical properties. The synthetic route is as follows. Quality Control of (3R,5S,6E)-7-[4-(4-Fluorophenyl)-6-isopropyl-2-[(methanesulfonyl) methylamino]pyrimidin-5-yl]-3,5-dihydroxyhept-6-enoic acid tert-butyl ester

Example 1; Hydrolysis of terf-butyl ester of rosuvastatin in aqueous solution of amines; 7.5 g of terf-butyl ester of rosuvastatin 38 ml of demineralized water 2 to 5 equivalents of amineThe reactants and water as the solvent are stirred in the autoclave from 98 to 1000C for 1 to 4 hours. The reaction mixture is sampled and analyzed by HPLC (“High Pressure Liquid Chromatography”) to find out the completion of reaction. Results are shown in Table 1. EPO

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, 355806-00-7, (3R,5S,6E)-7-[4-(4-Fluorophenyl)-6-isopropyl-2-[(methanesulfonyl) methylamino]pyrimidin-5-yl]-3,5-dihydroxyhept-6-enoic acid tert-butyl ester.

Reference:
Patent; LEK PHARMACEUTICALS D.D.; WO2006/136407; (2006); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 274693-26-4, name is 2-(((3aR,4S,6R,6aS)-6-(7-(((1R,2S)-2-(3,4-Difluorophenyl)cyclopropyl)amino)-5-(propylthio)-3H-[1,2,3]triazolo[4,5-d]pyrimidin-3-yl)-2,2-dimethyltetrahydro-3aH-cyclopenta[d][1,3]dioxol-4-yl)oxy)ethanol, the common compound, a new synthetic route is introduced below. Formula: C26H32F2N6O4S

a, preparation of crude ticagreride: 56gIsopropyl ticagreIntermediate(0.1 mol, 1.0 eq) was placed in 500 mL of dichloromethane and stirred to dissolve;1.1 g of trifluoroacetic acid (0.01 mol, 0.1 eq) was added dropwise at 0-5 C.The dichloromethane solution was dripped in 30 minutes; after the dropwise addition, the reaction was carried out at 5-10 C.The reaction was monitored by TLC; after 1 hour, TLC showed the reaction of the starting material was completed and 200 mL of water was added.The pH was adjusted to 6-7 with potassium carbonate, and the aqueous layer was extracted with dichloromethane (200 mL×2). The organic phase was combined and then water (300 mL×2).Wash with saturated brine (300 mL × 2), dry over anhydrous sodium sulfate, and filter.Evaporated to dryness under reduced pressure to give 45.8 g of crude ticagrei, yield 88%b, the preparation of ticagrelor amorphous: take 10g crude ticagrei,Placed in 100 ml of tetrahydrofuran solvent, stirred, and warmed to 65-70 C,Maintain this temperature for 30 min, add 1 g of activated carbon, stir for 10 min, filter with hot heat, rinse the filter cake with tetrahydrofuran, and gradually cool the filtrate to 30-35 C with stirring.Then slowly distill off the solvent under reduced pressure, and recycle the tetrahydrofuran.Made a foamy solid, crushed, dried,9.8 g of ticagrelor amorphous product was obtained.Its X-ray powder diffraction pattern is shown in Figure 1.

The synthetic route of 274693-26-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Nantong Changyou Pharmaceutical Technology Co., Ltd.; Li Zebiao; Ding Haiming; Zhang Qinghai; Li Keying; Tang Rongjie; Lin Yanfeng; (7 pag.)CN110183436; (2019); A;,
Pyrimidine | C4H4N2 – PubChem,
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