09/15/21 News New downstream synthetic route of 2972-52-3

At the same time, in my other blogs, there are other synthetic methods of this type of compound,2972-52-3, 2,4-Dichloro-5-pyrimidinecarbonyl chloride, and friends who are interested can also refer to it.

Reference of 2972-52-3, 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. 2972-52-3, name is 2,4-Dichloro-5-pyrimidinecarbonyl chloride. A new synthetic method of this compound is introduced below.

Methyl 2-(butYlaminoV4-(((tra^^ (0734) (0735) To a solution of 2,4-dichloropyrimidine-5-carbonyl chloride (500 mg, 2.38 mmol) in dichloromethane (30 mL) was added methanol (87.6 mg, 2.73 mmol) and diisopropylethylamine (369 mg, 2.86 mmol) at 0 °C. The resulting mixture was stirred for 1 h at 0 °C. Then the solvent was removed. The residue (461mg, 94percent) was dissolved in IP A (20 mL) and followed by the addition of tra5′-4-aminocyclohexanol (301.6 mg, 2.62 mmol) then DIEA (461.4 mg, 3.57 mmol) dropwisely. The resulting mixture was stirred at 0 °C for 90 min. After which butylamine (208.8 mg, 2.86 mmol) was added, followed by DIEA (461.4 mg, 3.57 mmol). The resulting mixture was stirred at room temperature for 3 h. Water was then added. The resulting mixture was extracted with EtOAc (3X). The combined organic layers were dried filtered and concentrated. The residue was purified on ISCO to provide methyl 2-(butylamino)-4-(((traj,-4-hydroxycyclohexyl)amino)pyrimidine-5 – carboxylate (682.6 mg, 89percent over 3 steps). 1H NMR (400 MHz, CDC13) delta 9.21 (s, 1H), 8.77 (s, 1H), 6.29 (s, 1H), 4.81-4.64 (m, 1H), 4.51 (s, 3H), 4.46-4.38 (m, 1H), 4.13-4.11 (m, 2H), 2.89-2.81 (m, 2H), 2.74 (d, J = 9.7 Hz, 2H), 2.35-2.25 (m, 2H), 2.23-2.00 (m, 6H), 1.67 (t, J = 7.2 Hz, 3H); 13C NMR (101 MHz, CDC13) delta 167.9, 162.5, 161.3, 160.3, 95.5, 69.7, 51.2, 48.3, 41.1, 33.8, 31.7, 30.3, 20.1, 13.8; MS m/z 323.20 [M+H]+.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,2972-52-3, 2,4-Dichloro-5-pyrimidinecarbonyl chloride, and friends who are interested can also refer to it.

Reference:
Patent; THE UNIVERSITY OF NORTH CAROLINA AT CHAPEL HILL; WANG, Xiaodong; ZHANG, Weihe; FRYE, Stephen; WO2015/157127; (2015); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

10 Sep 2021 News Introduction of a new synthetic route about 2972-52-3

According to the analysis of related databases, 2972-52-3, the application of this compound in the production field has become more and more popular.

Electric Literature of 2972-52-3, 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. 2972-52-3, name is 2,4-Dichloro-5-pyrimidinecarbonyl chloride, molecular formula is C5HCl3N2O, 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.

Ethyl 2,8,9J0J7J9.22-heptaazatricvclori6.3.1. .l0ltricosa-l(2U (23 8 8(22I19- entaene-21 -carboxylate (1279) (1280) A solution of 2,4-dicMoropyrirnidine-5-carbonyl chloride (1.00 g, 4.76 mmol) in ethanol (6.0 mL) was added DIPEA (2.5 mL, 14.4 mmol) slowly at 0 C under nitrogen. After 30 min, hex-5-yn-l -amine (0.476 g, 4.91 mmol) was added in one portion. The reaction mixture was stirred at room temperature for 3.5 h, then was added drop wise to a solution of 6-azidohexan-l -amine (0.801 g, 5.64 mmol) in ethanol (4.0 mL) at 50 C. After the reaction was complete (monitored by LCMS), the mixture was diluted with water (10 mL) and concentrated under a reduced pressure and filtered. The yellow solid was washed with water and dried under vacuum to be used in the next step without further purification (0.723 g, 39% over 3 steps).

According to the analysis of related databases, 2972-52-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; THE UNIVERSITY OF NORTH CAROLINA AT CHAPEL HILL; WANG, Xiaodong; ZHANG, Weihe; FRYE, Stephen; WO2015/157127; (2015); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

8 Sep 2021 News Brief introduction of 2972-52-3

Statistics shows that 2972-52-3 is playing an increasingly important role. we look forward to future research findings about 2,4-Dichloro-5-pyrimidinecarbonyl chloride.

Electric Literature of 2972-52-3, 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.2972-52-3, name is 2,4-Dichloro-5-pyrimidinecarbonyl chloride, molecular formula is C5HCl3N2O, molecular weight is 211.43, as common compound, the synthetic route is as follows.

2,4-dichIoro-2,4-(morpho A solution of 2,4-dichloropyrimidine-5-carbonyl chloride (422mg, 2,0 mmoi) in dichloromethane (10 mL) was added 4-(morpholinosulfonyl)aniline (508 nig. 2.1 mmoi) and DIEA (387 mg, 3.0 mmoi) at 0 C. The resulting mixture was stirred at 0 C for 1 h, Then, water was added. The resulting mixture was extracted with EtOAc (3x). The combined organic layers were dried (NaSO4), filtered and concentrated. The residue was purified on ISCO to give the title compound as a white solid (701.2 mg, 84%). 1H NMR (400 MHz, DMSO-d6) delta 1 1.98 – 1 1.90 (m5 I B), 8.29 (d, J = 6.4 Hz, IH), 7.89 (d, J = 8.8 Hz, 2H), 7.69 (d, J= 8.8 Hz, 2H), 3.65 – 3.56 (m, 4H), 2.87 – 2.78 (m, 4H); MS m/z 418,30 [M+H]+

Statistics shows that 2972-52-3 is playing an increasingly important role. we look forward to future research findings about 2,4-Dichloro-5-pyrimidinecarbonyl chloride.

Reference:
Patent; THE UNIVERSITY OF NORTH CAROLINA AT CHAPEL HILL; WANG, Xiaodong; ZHANG, Weihe; KIREEV, Dmitri; LIU, Jing; MCIVER, Andrew Louis; WO2014/85225; (2014); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Some scientific research about 2,4-Dichloro-5-pyrimidinecarbonyl chloride

The synthetic route of 2972-52-3 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. 2972-52-3, name is 2,4-Dichloro-5-pyrimidinecarbonyl chloride, the common compound, a new synthetic route is introduced below. category: pyrimidines

9.2: 2,4-Dichloropyrimidine-5-carboxylic Acid Ethyl Ester; In a 250 ml round-bottomed flask, under a nitrogen atmosphere, 13.5 g (64.0 mmol) of above compound are dissolved in 100 ml of anhydrous THF. 15 ml of absolute ethanol are added and the mixture is stirred for 10 min at ambient temperature. The mixture is diluted with a saturated aqueous solution of K2CO3 (100 ml) and extracted with ethyl acetate (4×100 ml). The organic phases are combined and then washed with 150 ml of a saturated aqueous solution of NaCl. After separation, the organic phase is dried over MgSO4 and filtered, and the solvent is evaporated off under reduced pressure, so as to obtain 14.0 g (63.3 mmol) of compound in the form of an orange oil. Yield=99%. 1H NMR DMSO d6 (300 MHz): 1.34 (t, J=7.1 Hz, 3H); 4.37 (q, J=7.1 Hz, 2H); 9.16 (s, 1H).

The synthetic route of 2972-52-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SANOFI-AVENTIS; US2011/251194; (2011); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

The origin of a common compound about 2,4-Dichloro-5-pyrimidinecarbonyl chloride

According to the analysis of related databases, 2972-52-3, the application of this compound in the production field has become more and more popular.

Electric Literature of 2972-52-3, 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. 2972-52-3, name is 2,4-Dichloro-5-pyrimidinecarbonyl chloride, molecular formula is C5HCl3N2O, 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.

To a solution of 9 g (42.8 mmol) of 2,4-dichloro-5-pyrimidinecarboxylic acid chloride (Manchester Organics Limited) in 60 mL of ether are added 10 mL of water and the reaction mixture is stirred vigorously at 35 C. for 1 hour. After addition of ether and separation of the phases by settling, the organic phase is dried over Na2SO4, filtered and concentrated under vacuum. 7.7 g of a colourless oil that solidifies rapidly in air, and which is used immediately in the following step, are obtained. Yield=93%.

According to the analysis of related databases, 2972-52-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; SANOFI; US2012/277220; (2012); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

The origin of a common compound about 2,4-Dichloro-5-pyrimidinecarbonyl chloride

With the rapid development of chemical substances, we look forward to future research findings about 2972-52-3.

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. 2972-52-3, name is 2,4-Dichloro-5-pyrimidinecarbonyl chloride, molecular formula is C5HCl3N2O, 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. Recommanded Product: 2,4-Dichloro-5-pyrimidinecarbonyl chloride

Example 18Synthesis of 5-Carboxyamide-2,4-DichloropyrimidineConcentrated ammonium hydroxide solution in H2O (assumed to be 8.5M; 14.1 mL; 120 mmol) was added over 15-20 minutes to a stirred solution of 2,4-dichloropyrimidine-5-carbonyl chloride (12.5 g; 60 mmol; Manchester Organics, Sutton Weaver, England) in CH2Cl2 (300 mL) at -15 to -20 C. (internal temperature) [n.b.: a precipitate is formed during the addition]. After complete addition, the mixture was filtered (the filter cake comprises desired product and an impurity-for purification see below). H2O (50 mL) was added to the filtrate, which was partitioned. The organic layer was dried (NaSO4), filtered and the solvent removed under vacuum to give the title compound (1.1 g) as a solid. The filter cake from above was triturated with hot (ca. 50 C.) EtOAc (300 mL) and the mixture filtered-this was repeated another 2 times. The combined filtrates from the trituration were concentrated under vacuum to give another 9.1 g of the title compound. The total yield from the reaction is 10.2 g (88%). Data identical to those of Example 17.

With the rapid development of chemical substances, we look forward to future research findings about 2972-52-3.

Reference:
Patent; Singh, Rajinder; Tso, Kin; Zhang, Jing; Duncton, Matthew; Alvarez, Salvador; Kolluri, Rao; Ramphal, John; Holland, Sacha; US2011/130415; (2011); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Analyzing the synthesis route of 2,4-Dichloro-5-pyrimidinecarbonyl chloride

According to the analysis of related databases, 2972-52-3, the application of this compound in the production field has become more and more popular.

Related Products of 2972-52-3, 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 2972-52-3, name is 2,4-Dichloro-5-pyrimidinecarbonyl chloride. This compound has unique chemical properties. The synthetic route is as follows.

To a solution of 2,4-dichloropyrimidine-5-carbonyl chloride (500 mg, 2.38 mmol) in dichloromethane (30 mL) was added methanol (87.6 mg, 2.73 mmol) and diisopropyeihylamine (369 mg, 2,86 mmol) at 0 C. The resulting mixture was stirred for 1 h at 0 C. Then the solvent was removed. The residue (461rng, 94%) was dissolved in IPA (20 ml,) and followed by the addition of trans-4-aminocyclohexanol (301.6 mg, 2.62 mmol) then DIEA (461.4 mg, 3.57 mmol) dropwiseiy. The resulting mixture was stirred at 0 C for 90 min. After which buiyiamine (208,8 mg, 2.86 mmol) was added, followed by DIEA (461.4 mg., 3.57 mmol). The resulting mixture was stirred at room temperature for 3 h. Water was then added. The resulting mixture was extracted with EtOAc (3X). The combined organic layers were dried (Na2SO4, filtered and concentrated. The residue was purified on ISCO to give methyl 2-(butylamino)-4-((trans-4-hydroxycyclohexyl)amino)pyrimidine-5-carboxylate (682.6 mg, 89% over 3 steps). 1H NMR (400 MHz, CDCl3) delta 9.21 (s, 1H), S.77 (s, 1H), 6.29 (s, 1H), 4.81 – 4.64 (m, 1H), 4.51 (s, 3H), 4.46-4.38 (m, 1H), 4.13-4.1 (m, 2H), 2.89-2.81 (m, 2H), 2.74 (d, J – 9.7 Hz, 2H), 2.35 – 2.25 (m, 2H), 2.23 – 2.00 (m, 6H), 1 ,67 (t, J- 7.2 Hz, 3H); 13C NMR (101 MHz, CDCl3) delta 167.9, 162,5, 161.3, 160.3, 95.5, 69.7, 51.2, 48.3, 41. L 33.8, 31 ,7, 30.3, 20.1, 13,8; MS m/z 323.20 [M+H]+

According to the analysis of related databases, 2972-52-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; THE UNIVERSITY OF NORTH CAROLINA AT CHAPEL HILL; WANG, Xiaodong; ZHANG, Weihe; KIREEV, Dmitri; LIU, Jing; MCIVER, Andrew Louis; WO2014/85225; (2014); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Some tips on 2,4-Dichloro-5-pyrimidinecarbonyl chloride

According to the analysis of related databases, 2972-52-3, the application of this compound in the production field has become more and more popular.

Reference of 2972-52-3, 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. 2972-52-3, name is 2,4-Dichloro-5-pyrimidinecarbonyl chloride, molecular formula is C5HCl3N2O, 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.

Example 3 Synthesis of 5-carboxyamide-2,4-dichloropyrimidine To a 2 L round bottom flask equipped with water condenser and a CaCl2 drying tube, 2,4-dihydroxypyrimidine (25 g, 0.16 mole) was added to PCl5 (117 g, 0.56 mole), and POCl3 (250 ml, 2.6 mole). The mixture was heated at 115 C. overnight to give a clear, slightly light yellow solution. The mixture was cooled to room temperature, and was concentrated under reduced pressure to give pale yellowish oil. To this oil, anhydrous 1,4-dioxane (300 ml) was added and the mixture was cooled to 0 C. in an ice/water bath. 35 ml of NH3 in water (28%) was added dropwise to the mixture with stirring, temperature was kept below 5 C. The mixture changed from clear to white with precipitate forming, and was stirred for 1 hour at 0 C., reaction was followed by TLC (1:1 Hexanes:Ethyl Acetate). Ethyl acetate (700 ml) and water (500 ml) were added to the mixture, the 2 layers were separated. The organic layer was dried with Na2SO4, and filtered. The solution was concentrated under reduced pressure to give a light yellow solid. This light yellow solid was sonicated with methylene chloride (200 ml), and filtered to give a pale yellow solid (16 g). This pale yellow solid was dissolved into ethyl acetate (1.5 L) and washed with sat. NaHCO3 (500 ml). The organic layer was dried with Na2SO4, filtered, and concentrated under reduced pressure to give 13.1 g of product as a white solid (44% yield). 1H NMR (DMSO-d6, 300 MHz): delta 8.86 (s, 1H), 8.14 (bs, 1H), 8.02 (bs, 1H).

According to the analysis of related databases, 2972-52-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Holland, Sacha; Kolluri, Rao; Alvarez, Salvador; Duncton, Matthew; Singh, Rajinder; Zhang, Jing; Masuda, Esteban; US2012/22092; (2012); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Analyzing the synthesis route of 2,4-Dichloro-5-pyrimidinecarbonyl chloride

Statistics shows that 2972-52-3 is playing an increasingly important role. we look forward to future research findings about 2,4-Dichloro-5-pyrimidinecarbonyl chloride.

Electric Literature of 2972-52-3, 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.2972-52-3, name is 2,4-Dichloro-5-pyrimidinecarbonyl chloride, molecular formula is C5HCl3N2O, molecular weight is 211.43, as common compound, the synthetic route is as follows.

Amberlyst A-21 ion exchange resin (1. 8 g) was added to a solution of 2,4- DICHLOROPYRIMIDINE-5-CARBONYL chloride (18.3 g, 86. 6 mmol) in ethyl acetate (400 mL). More ethyl acetate (50 mL) was added and 2,6-dimethylaniline (10.5 g, 10.7 mL, 86. 6 mmol) was added dropwise at room temperature. The reaction mixture was heated at 50 C overnight then cooled and quenched with water and extracted extracted with ethyl acetate (3 x 100 mL). The organic layer was washed with 1 N HC1 (30 mL), 1 M NaOH (30 mL) and brine (30 mL). The organic layer was then dried on sodium sulfate, filtered and concentrated in vacuo. The crude product was washed with dichloromethane (2 X 30 ML) to afford the title compound as a pale yellow solid NMR (400 MHz, CDC13) : 9. 08 (1H, s), 7.71 (1H, s), 7.15-7. 23 (3H, m), 2.32 (6H, s); 13C NMR (400 MHz, CDC13) : 19.12, 127.56, 128. 78, 129.00, 132.75, 135.81, 158. 61,160. 25,162. 23,162. 41; MS: 296 [M+H+]

Statistics shows that 2972-52-3 is playing an increasingly important role. we look forward to future research findings about 2,4-Dichloro-5-pyrimidinecarbonyl chloride.

Reference:
Patent; AMGEN INC.; WO2005/9443; (2005); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Some scientific research about 2972-52-3

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 2972-52-3, 2,4-Dichloro-5-pyrimidinecarbonyl chloride.

Reference of 2972-52-3, 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 2972-52-3, name is 2,4-Dichloro-5-pyrimidinecarbonyl chloride. This compound has unique chemical properties. The synthetic route is as follows.

100 g of 2,4-dichloro-5-pyrimidinyl chloride is dissolved in 800 g of anhydrous chloroform,Add 95 grams of triethylamine, lower the temperature to 0 C, and add 38 grams of tert-butylamine dropwise.After the addition, the reaction was held at 0 C for 1 hour.100 g of compound 2,4-dichloro-5-pyrimidine tert-butyramide was obtained by filtration,The measured purity is greater than 98% and the yield is 85%;

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 2972-52-3, 2,4-Dichloro-5-pyrimidinecarbonyl chloride.

Reference:
Patent; Nanjing Puruida Pharmaceutical Technology Co., Ltd.; Wang Xiaobo; (7 pag.)CN110452179; (2019); A;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia