Simple exploration of 5750-76-5

Statistics shows that 5750-76-5 is playing an increasingly important role. we look forward to future research findings about 2,4,5-Trichloropyrimidine.

With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.5750-76-5, name is 2,4,5-Trichloropyrimidine, molecular formula is C4HCl3N2, molecular weight is 183.4231, as common compound, the synthetic route is as follows.5750-76-5

2,4,5-Trichloropyrimidine (250 mg, 1.36 mmol) and ferric acetylacetonate (24 mg, 0.07 mniol) were taken up in tetrahydroruran (2.7 ml) and the reaction was cooled to -78 C.Methylmagnesium bromide (0.45 ml of 3 M in THF, 1.36 mmol) was added dropwise and the mixture was stirred at -78 C for one hour. The mixture was quenched with aqueous ammonium chloride and extracted with ethyl acetate. The combined organic fractions were dried over magnesium sulfate, filtered, and the solvent was evaporated under reduced pressure. The resulting residue was purified by Combiflash (0-10% diethylether in hexanes) to provide 2,5- dichloro-4-methylpyrimidine (99 mg, 0.61 mmol, 45 %) as a white solid. MS APCI: [M+H]+ m/z 163.0.

Statistics shows that 5750-76-5 is playing an increasingly important role. we look forward to future research findings about 2,4,5-Trichloropyrimidine.

Reference:
Patent; MERCK SHARP & DOHME CORP.; MERCK CANADA INC.; ALTMAN, Michael, D.; ARRINGTON, Kenneth, L.; BURCH, Jason; COTE, Bernard; FOURNIER, Jean-Francois; GAUTHIER, Jacques, Yves; KATTAR, Solomon; KNOWLES, Sandra Lee; LIM, Jongwon; MACHACEK, Michelle, R.; NORTHRUP, Alan, B.; REUTERSHAN, Michael, H.; ROBICHAUD, Joel, S.; SCHELL, Adam, J.; SPENCER, Kerrie, B.; WO2011/75560; (2011); A1;,
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Some tips on 302964-08-5

The chemical industry reduces the impact on the environment during synthesis 302964-08-5, I believe this compound will play a more active role in future production and life.

In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 302964-08-5 as follows., 302964-08-5

62.5 mL of 3-methylbutan-l-ol was charged into 4 necked RBF at ~ 25 C. 2.5 g of N-(2-chloro-6-methylphenyl)-2-[6-chloro-2-methyl-4-pyrimidinyl) amino]-5-thiazole carboxamide and 4.12 g of 1-(3-Hydroxy)ethylpiperazine were added to the reaction mixture. The reaction mass was stirred for ~ 15 mins and then the temperature of reaction mass was raised to 135 C. After stirring the heated reaction mass (along with continuous reaction monitoring), the reaction mass was slowly cooled to 25 C, in 2 h. The cooled reaction mass was then stirred for 5 h, filtered and washed with 5.0 mL 3-methylbutan-l-ol. The material obtained after washing was suck dried for 15 min. The partially wet material obtained above was charged into a RBF and 48.75 mL 3- methylbutan-l -ol, 73 mg Diisopropylethylamine (DIPEA) and 70 mg 2-bromo ethanol were added to the reaction mixture. The reaction mixture was then heated to ~80C, wherein stirring was performed for 12 h. After stirring, the reaction mass was allowed to slowly cool down to -25 C, wherein it was again stirred for 1 h. Then the reaction mass was filtered and washed with 6.5 mL of 3-methylbutan-l-ol. The wet material obtained was unloaded, air dried for 30 min and then vacuum dried for 10 h at 65 C. The material was then allowed to cool down to 25 C and unloaded to obtain 3.0 g crystalline Form-SDI of Dasatinib having XRPD pattern according to Fig-1 , IR spectrum according to Fig-2 and DSC pattern according to Fig- 3. Yield: 83 % % purity (By HPLC): 99.42 % 1H NMR (400 MHz, DMSO) delta 11.39 (s, 1H), 9.8 (s, 1H), 8.22 (s, 1H), 7.4 (dd, 2H), 7.2 (m, 1H), 6.04 (s, 1H), 4.4 (t, 1H), 3.4 (m, 6H), 2.44 (m, 3H), 2.4 (m, 3H), 2.41 (s, 3H), 2.2 (s, 3H), 1.6 (sep, 1H), 1.3 (q, 2H), 0.85 (d, 6H).

The chemical industry reduces the impact on the environment during synthesis 302964-08-5, I believe this compound will play a more active role in future production and life.

Reference:
Patent; SHILPA MEDICARE LIMITED; SRIRAM, Rampalli; PRADEEP, Pothana; SURESH, Garbapu; PRASHANT, Purohit; AKSHAY KANT, Chaturvedi; WO2015/68055; (2015); A1;,
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Introduction of a new synthetic route about 32779-36-5

The synthetic route of 32779-36-5 has been constantly updated, and we look forward to future research findings.

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. 32779-36-5, name is 5-Bromo-2-chloropyrimidine, the common compound, a new synthetic route is introduced below. 32779-36-5

Preparation B: N- j5-(4-bromophenyl)-6- j2- j(5-bromo-2-pyrimidinyl)oxyj ethoxyj – 4-pyrimidinylj -N?- propylsulfamide (macitentan):N-(5 -(4-bromophenyl)-6-(2-hydroxyethoxy)pyrimidin-4-yl)propane- 1 -sulfamide (200 g; 0.46 mol; see Example 2 or 3) and 5-bromo-2-chloropyrimidine (117 g; 0.60 mol; 1.3 eq) were dissolved in toluene (3 L) and DMF (400 mL). The reaction mixture was warmed up to 50¡ãC and toluene (approx. 400 mL) was distilled our under reduced pressure. The mixture was cooled to 0 ¡ãC and tBuOK (156 g, 3 eq, 1.38 mol) was added portionwise. It was stirred at 20 ¡ãC for 1 h. Water (1 L) was added and the pH of the solution was adjusted to 3-5 using 33percent aq. HC1. The mixture was heated to 50¡ãC and the layers were separated. The org. phase was treated with charcoal at 50¡ãC and filtered over Celite. The filter cake was rinsed with toluene. At 50¡ãC, water (1 L) was added to the org. layer. The layers were separated. The org. layer was concentrated under reduced pressure to a total volume of 1 L and cooled to 0¡ãC. The solid obtained was filtered off It was rinsed with toluene and MeOH. The crude material was suspended in EA (1 L) and heated to 50¡ãC. 300 mL of EA were distilled out and MeOH (400 mL) was added. The suspension was cooled down to 0¡ãC. The solid was filtered off, rinsed with MeOH and dried under reduced pressure to afford the title compound as a white solid (225 g; 83percent yield).

The synthetic route of 32779-36-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ACTELION PHARMACEUTICALS LTD; ABELE, Stefan; FUNEL, Jacques-Alexis; SCHINDELHOLZ, Ivan; WO2014/155304; (2014); A1;,
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Some scientific research about 7752-82-1

Statistics shows that 7752-82-1 is playing an increasingly important role. we look forward to future research findings about 5-Bromopyrimidin-2-amine.

With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.7752-82-1, name is 5-Bromopyrimidin-2-amine, molecular formula is C4H4BrN3, molecular weight is 173.9987, as common compound, the synthetic route is as follows.7752-82-1

c) 6-Bromo-imidazo[1,2-a]pyrimidine; 50 mmol of 5-bromo-pyrimidin-2-ylamine are dissolved in 200 mi of saturated aqueous sodium hydrogencarbonate solution. 55 mmol of chloroacetaldehyde are added to the reaction mixture and the mixture is stirred for 24 hours at 25C. The mixture is extracted with ethyl acetate (3×300 mi) and the combined extracts are dried over sodium sulphate and evaporated under reduced pressure. Flash chromatography (Si02 60F) of the residue provides the title compound which is identified on the basis of its Rf-value.

Statistics shows that 7752-82-1 is playing an increasingly important role. we look forward to future research findings about 5-Bromopyrimidin-2-amine.

Reference:
Patent; SPEEDEL EXPERIMENTA AG; WO2005/90305; (2005); A1;,
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The origin of a common compound about 137281-39-1

According to the analysis of related databases, 137281-39-1, the application of this compound in the production field has become more and more popular.

137281-39-1 , The common heterocyclic compound, 137281-39-1, name is 4-(2-(2-Amino-4-oxo-4,7-dihydro-1H-pyrrolo[2,3-d]pyrimidin-5-yl)ethyl)benzoic acid, molecular formula is C15H14N4O3, 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.

General procedure: To a suspension of compound 6 (0.033 mmol) in N,N-dimethylformamide (5 mL), corresponding amine (RNH2) (0.033 mmol) and DIPEA (0.1 mmol) were added at about 10 C under nitrogen atmosphere. To this, diethylphosphorocyanidate(0.04 mmol) was added slowly over a period of 15 min. The resultant solution was stirred for 3 h at about 10 C. The reaction was complete by TLC (TLC system: 10% methanol in chloroform). Reaction was slowly quenched using saturated sodium-bi-carbonate solution and the resulted solid was stirred for 30min. Solid was collected by filtration and the wet cake was washed with saturated sodium-bi-carbonate solution. Upon drying the wet cake for an hour under vacuum, it was further suspended in methanol and stirred for 30 min, filtered, collected and dried to get respective pure compounds.

According to the analysis of related databases, 137281-39-1, the application of this compound in the production field has become more and more popular.

Reference:
Article; Balaraman, Selvakumar; Nayak, Nagaraj; Subbiah, Madhuri; Elango, Kuppanagounder P.; Medicinal Chemistry Research; vol. 27; 11-12; (2018); p. 2538 – 2546;,
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New learning discoveries about 591-55-9

Statistics shows that 591-55-9 is playing an increasingly important role. we look forward to future research findings about 5-Aminopyrimidine.

The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a compound 591-55-9, name is 5-Aminopyrimidine. This compound has unique chemical properties. The synthetic route is as follows. 591-55-9

To a solution of (9S)-2-(2-(trifluoromethyl)pyridin-4-yl)-7,8,9,10-tetrahydro-6H-5,9-methanopyrido[2,3-b][1,4]diazocine (0.5 g, 1.561 mmol), triethylamine (0.653 mL, 4.68 mmol) in THF (10 mL) was added bis(trichloromethyl) carbonate (0.232 g, 0.780 mmol) at 25 C. under nitrogen atmosphere and stirred at RT for 30 min. Then pyrimidin-5-amine (0.445 g, 4.68 mmol) was added and heated the reaction mixture at 65 C. for 16 h. Allowed to cool to RT and solvent was removed on rota-vapour, the crude was diluted with CH2Cl2 (20 ml) and washed with water (5 ml), brine solution (5 ml) followed by dried over sodium sulfate. The organic solvent was evaporated under reduced pressure to obtain the crude product. The crude mixture was purified by prep-HPLC (formic acid, ACN 25%) to afford (9S)-N-(pyrimidin-5-yl)-2-(2-(trifluoromethyl)pyridin-4-yl)-8,9-dihydro-6H-5,9-methanopyrido[2,3-b][1,4]diazocine-10(7H)-carboxamide (250 mg, 0.56 mmol, 45% yield) as an off white solid (TLC: 80% EtOAc in Hexane, Rf: 0.5), LCMS (m/z): 442.3 [M+H]+. 1H NMR (400 MHz, DMSO-d6): delta 13.07 (s, 1H), 9.08-8.72 (m, 4H), 8.38 (dd, J=1.7, 0.9 Hz, 1H), 8.28 (dd, J=5.2, 1.6 Hz, 1H), 7.90 (d, J=8.0 Hz, 1H), 7.79 (d, J=8.0 Hz, 1H), 4.85 (t, J=2.7 Hz, 1H), 3.43 (dd, J=13.7, 1.9 Hz, 1H), 3.33 (d, J=10.1 Hz, 2H), 2.91 (d, J=13.7 Hz, 1H), 2.15-1.79 (m, 2H), 1.33 (s, 2H).

Statistics shows that 591-55-9 is playing an increasingly important role. we look forward to future research findings about 5-Aminopyrimidine.

Reference:
Patent; BLUM, Charles A.; Caldwell, Richard Dana; Casaubon, Rebecca; Disch, Jeremy S.; Fox, Ryan Michael; Koppetsch, Karsten; Miller, William Henry; NG, Pui Yee; Oalmann, Christopher; Perni, Robert B.; Szczepankiewicz, Bruce G.; White, Brian; US2015/152108; (2015); A1;,
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The important role of 1004-40-6

At the same time, in my other blogs, there are other synthetic methods of this type of compound,1004-40-6, 6-Amino-4-hydroxy-2-mercaptopyrimidine, and friends who are interested can also refer to it.

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. 1004-40-6, name is 6-Amino-4-hydroxy-2-mercaptopyrimidine. A new synthetic method of this compound is introduced below., 1004-40-6

General procedure: A mixture of freshly calcined K2CO3 (7.4 mmol), 2-thiouracil 2a-c (7.0 mmol), 2-(bromomethyl)-2-isoindole-1,3-dione (7.7 mmol), and anhydrous DMF (20 ml) was stirred at room temperature for 72 h. The reaction mixture was filtered, and the filtrate was evaporated to dryness. The obtained residue was taken up in 1 aqueous solution, the mixture was filtered, the filtrate was extracted with EtOAc (3¡Á50 ml), dried over MgSO4, filtered, and evaporated at reduced pressure. The solids collected by filtration were air-dried until constant mass, combined with the evaporated organic extract, and the obtained mixture was purified by preparative HPLC.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,1004-40-6, 6-Amino-4-hydroxy-2-mercaptopyrimidine, and friends who are interested can also refer to it.

Reference:
Article; Novakov, Ivan A.; Sheikin, Dmitry S.; Chapurkin, Viktor V.; Nawrozkij, Maksim B.; Babushkin, Alexande S.; Kuznetsov, Yaroslav P.; Ruchko, Evsey A.; Kachala, Vadim V.; Maryshev, Anton Yu.; Schols, Dominique; Chemistry of Heterocyclic Compounds; vol. 56; 1; (2020); p. 67 – 72; Khim. Geterotsikl. Soedin.; vol. 56; 1; (2020); p. 67 – 72,6;,
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A new synthetic route of 1500-85-2

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 1500-85-2, 7H-Pyrrolo[2,3-d]pyrimidin-4-amine, other downstream synthetic routes, hurry up and to see.

1500-85-2, 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. 1500-85-2, name is 7H-Pyrrolo[2,3-d]pyrimidin-4-amine, molecular formula is C6H6N4, 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.

7H-pyrrolo[2,3-d]pyrimidin-4-amine (0.4 g, 3.0 mmol) was dissolved in 10 mL DMF.NIS (0.74 g, 3.3 mmol) was added in portions under ice bath.After the feeding is completed, the ice bath is removed.The reaction was allowed to proceed at room temperature for 3 hours, and the reaction was confirmed to be complete by TLC. 20 mL of water was added to the reaction solution.It was extracted with ethyl acetate (30 mL*3), and the organic phase was washed with 20 mL of brine.Dry over anhydrous sodium sulfate, concentrate,The residue was separated into a pale yellow solid (0.56 g).The yield was 73%.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 1500-85-2, 7H-Pyrrolo[2,3-d]pyrimidin-4-amine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Shenzhen Tajirui Bio-pharmaceutical Co., Ltd.; Wang Yihan; Xing Qingfeng; (59 pag.)CN110194772; (2019); A;,
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Brief introduction of 504-17-6

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 504-17-6, 4,6-Dihydroxy-2-mercaptopyrimidine, other downstream synthetic routes, hurry up and to see.

504-17-6, 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. 504-17-6, name is 4,6-Dihydroxy-2-mercaptopyrimidine, molecular formula is C4H4N2O2S, 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.

General procedure: A mixture of an aldehyde (0.25 mmol), 2-thiobarbituric acid (0.5 mmol), ammonium acetate (0.3 mmol), and CuFe2O4 (10 mol%), with distilled H2O, in an open tall beaker was irradiated inside microwave oven at 100 W for an appropriate time (monitored by TLC). After completion of the reaction, for removing the catalyst, the hot solution was filtrated with external magnetic for several times. The solvent was evaporated, and the precipitate was washed from ethanol and hot water to afford the pure product.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 504-17-6, 4,6-Dihydroxy-2-mercaptopyrimidine, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Naeimi, Hossein; Didar, Asieh; Rashid, Zahra; Journal of the Iranian Chemical Society; vol. 14; 2; (2017); p. 377 – 385;,
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Some tips on 1193-24-4

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 1193-24-4, 4,6-Dihydroxypyrimidine, other downstream synthetic routes, hurry up and to see.

1193-24-4, 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. 1193-24-4, name is 4,6-Dihydroxypyrimidine. A new synthetic method of this compound is introduced below.

EXAMPLES 1-6 General Procedure for Conversion of 4,6-dihydroxypyrimidine (DHP) to 4,6-dichloropyrimidine (DCP): The reaction vessel is a Morton-type flask fitted with a heating mantle, a mechanical agitator, a temperature probe, a phosgene dip pipe (which also serves as a nitrogen inlet when phosgene is not being introduced to the reactor), and a dry ice condenser. The dry ice condenser is vented into a caustic scrubber. The reactor is charged with 4,6-dihydroxypyrimidine, solvent, and catalyst, forming a slurry. The agitator is started and the mixture is heated to 105-110 C. When this temperature range is reached, phosgene gas is introduced subsurface to the reaction mixture via the dip pipe. Phosgene addition is continued over 3-5 hours. During the addition, phosgene escaping the reaction is condensed by the dry ice condenser and returned to the reactor. This reflux of phosgene begins shortly after the phosgene addition is begun, and continues throughout the course of the reaction.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 1193-24-4, 4,6-Dihydroxypyrimidine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Doyle, Timothy John; Wehrenberg, Peter Karl; Standen, Michael Charles Henry; US2002/42514; (2002); A1;,
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