Day: November 2, 2020

118-70-7, 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 118-70-7 as follows.

10 mL of formamide and 90 g of 4,5,6-triaminopyrimidine (Formula 6) were added to a 1000 mL reaction flask and heated to 140 to 150 C for 4 hours. The reaction was completed and cooled to a temperature of 25 to 15 C Crystallization, filtration, formamide rinsing, water elution, gray adipate crude, refined with water, activated carbon decolorization after 79.5g white crystalline powder adenine (Formula 1), yield 81.8%, HPLC 99.9%.

The chemical industry reduces the impact on the environment during synthesis 118-70-7, I believe this compound will play a more active role in future production and life.

Reference:
Patent; Taizhou Xingming Pharmaceutical Co., Ltd.; Liu Yi; Zhao Wujie; (10 pag.)CN106749043; (2017); A;,
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. 63234-80-0, name is 3-(2-Chloroethyl)-2-methyl-6,7,8,9-tetrahydro-4H-pyrido[1,2-a]pyrimidin-4-one, the common compound, a new synthetic route is introduced below. 63234-80-0

General procedure: A creamy white solid of 3-(2-chloroethyl)- 2-methyl-6,7,8,9-tetrahydro-4H-pyrido[1,2-a] pyrimidin-4-one (5) (1.0eq) in N,N-dimethylformamide was taken, pottasium carbonate (3.0 eq) was added to the reaction mixture and then the appropriate aliphatic/ aromatic/heterocyclic amines (1.0 eq) were added and the reaction mixture was heated at 80 ¡ãC for 8h. The progress of the reaction was monitored by TLC. Upon completion, the solvent was removed by water wash and extracted with ethyl acetate. The organic layer was washed with 10percent ammonium chloride solution and finally water wash was given to organic layer and dried with anhydrous sodium sulphate. The solvent was evaporated to get crude product which was purified by column chromatography over silica gel (60-120mesh) using hexane: ethyl acetate(8:2) as an eluent.

The synthetic route of 63234-80-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Krishnamurthy, Byregowda; Vinaya, Kambappa; Rakshith, Devraj; Prasanna, Doddakunche Shivaramu; Rangappa, Kanchugarakoppal Subbegowda; Medicinal Chemistry; vol. 9; 2; (2013); p. 240 – 248;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

The common heterocyclic compound, 32779-36-5, name is 5-Bromo-2-chloropyrimidine, molecular formula is C4H2BrClN2, 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. 32779-36-5

Step 1. 5-Bromo-N-cyclopropylpyrimidin-2-amine A solution of 5-bromo-2-chloropyrimidine (3.87 g, 20 mmol) and cyclopropylamine (5.7 g, 0.1 mol) in 20 mL THF was heated at 65¡ã C. for 5 hrs in a sealed tube. The mixture was evaporated in vacuo, to the residue ethanol was added, after filtration, the cake was washed with ethanol to give 4.07 g product as a colorless solid (95.5percent). 1H NMR (300 MHz, CDCl3) delta: 8.32 (2H, s), 5.58 (1H, brs), 2.72 (1H, brs), 0.82-0.84 (2H, m), 0.54 (2H, brs). LCMS: m/z [M+H]+ 214.0011.

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

Reference:
Patent; Astar Biotech LLC; YU, Chunrong; Huang, Haihong; Zhang, Dongfeng; Li, Peng; US2014/31354; (2014); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

3740-92-9 , The common heterocyclic compound, 3740-92-9, name is 4,6-Dichloro-2-phenylpyrimidine, molecular formula is C10H6Cl2N2, 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.

EXAMPLE VIII Two grams of 4,6-dichloro-2-phenylpyrimidine is added in small portions to 10 ml. of N-methylpiperazine with slight warming and stirring. The resulting mixture is heated on a steam bath for several minutes, then poured into 250 ml. of water. The product (2.4 g., m.p. 81¡ã-87¡ãC.) is then recrystallized from n-pentane to afford 4-chloro-6-(4-methyl-1-piperazinyl)-2-phenylpyrimidine, m.p. 91¡ã-92.5¡ãC. Anal. for C15 H17 N4 Cl: Calcd. C, 62.38; H, 5.93; N, 19.40; Cl, 12.28. Found: C, 62.32; H, 5.65; N, 19.62; Cl, 12.1.

According to the analysis of related databases, 3740-92-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; American Home Products Corporation; US3940395; (1976); A;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

611-08-5 , The common heterocyclic compound, 611-08-5, name is 5-Nitrouracil, molecular formula is C4H3N3O4, 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.

Preparation of 2,4-dichloro-5-nitropyrimidine. 5-Nitrouracil, was treated with phosphorous oxychloride and N, N- [DIMETHYLANILINE,] according to the procedure of Whittaker (J. Chem. Soc. 1951,1565), to give the title compound, which is also available from City Chemical (West Haven, CT).

According to the analysis of related databases, 611-08-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ELAN PHARMACEUTICALS, INC.; WO2003/99231; (2003); A2;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

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 113583-35-0 as follows., 113583-35-0

Process for producing 3-[(4,6-dimethoxypyrimidin-2-yl)oxy]-6-methylaminopicolinic acid (Second method) 10.5 mg (0.0576 mmol) of methyl 6-methylamino-3-hydroxypicolinate, 11.6 mg (0.0532 mmol) of 2-methylsulfonyl-4,6-dimethoxypyrimidine, 8.8 mg (0.637 mmol) of potassium carbonate and 0.5 ml of dry dimethylsulfoxide were mixed. The mixture was stirred at room temperature for 5 hours, and then a 10% potassium hydroxide aqueous solution (corresponding to 90 mg, 0.160 mmol) was added thereto. The mixture was reacted at room temperature for one hour, and then 2.0 ml of water was added to the reaction mixture. Further, 1.0 ml of a 10% citric acid aqueous solution was added thereto, and the mixture was left to stand, whereby crystals precipitated. After being thoroughly precipitated, the crystals were filtered under suction and washed with water. The crystals were dried to obtain 3-[(4,6-dimethoxypyrimidin-2-yl)oxy]-6-methylaminopicolinic acid. Colorless prism crystals, 13.7 mg (yield: 84.0%)

The chemical industry reduces the impact on the environment during synthesis 113583-35-0, I believe this compound will play a more active role in future production and life.

Reference:
Patent; Kumiai Chemical Industry Co., Ltd.; Ihara Chemical Industry Co., Ltd.; US5403816; (1995); A;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

32779-36-5, 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. 32779-36-5, name is 5-Bromo-2-chloropyrimidine, molecular formula is C4H2BrClN2, 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.

Synthesis of Compound 11-3 (0400) To a solution of 11-2 (2.0 g, 10 mmol) in methanol (15 mL) was added CH3ONa (2.16 g, 40 mmol). The resulting mixture was stirred at 70 C. overnight. Methanol was evaporated in vacuum. Water (10 mL) was added carefully to the residue and the mixture was extracted with ethyl acetate (300 mL¡Á3). The combined organic layers were dried over Na2SO4, filtered and concentrated to afford 11-3 as a yellow solid (1.17 g, 60%).

The chemical industry reduces the impact on the environment during synthesis 32779-36-5, I believe this compound will play a more active role in future production and life.

Reference:
Patent; Nivalis Therapeutics, Inc.; Wasley, Jan; Rosenthal, Gary J.; Sun, Xicheng; Strong, Sarah; Qiu, Jian; US9138427; (2015); B2;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

The common heterocyclic compound, 213265-83-9, name is 4,6-Dichloro-5-fluoropyrimidine, molecular formula is C4HCl2FN2, 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. 213265-83-9

0.2 g of 4,6-dichloro-5-fluoropyrimidine and 0.41 g of 3,5-dimethylpiperidine (cis/trans diastereomer = about 3/1) were mixed and left for 30 minutes at room temperature. The reaction mixture was subjected to silica gel column chromatography to obtain 0. 1 g of 4-CHLORO-6- (CIS-3, 5-dimethyl piperidino) -5-fluoropyrimidine and 0.05 g of 4-chloro- 6- (TRANS-3, 5-dimethylpiperidino) pyrimidin. cis diastereomer: H-NMR : 0.84 (dd, 1H), 0.93 (d, 6H), 1.64-1. 78 (m, 2H), 1.84-1. 92 (m, 1H), 2.46 (dd, 2H), 4.48 (d, 2H), 8. 11 (s, 1H) trans diastereomer: H-NMR : 0.96 (d, 6H), 1.51 (t, 2H), 1.96-2. 06 (m, 2H), 3.40 (dd, 2H), 3.83 (dd, 2H), 8. 10 (s, 1H)

The synthetic route of 213265-83-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SUMITOMO CHEMICAL COMPANY, LIMITED; WO2004/99160; (2004); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Some common heterocyclic compound, 5750-76-5, molecular formula is C4HCl3N2, 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.5750-76-5

In Scheme 2In the synthesis of Compound 2-5,The starting material 2-fluoronitrobenzene (i.e., compound 2-1)The remaining synthetic methods were the same as those of Scheme 1 of Scheme 1,To give compound 2-5, yield: 33%.In the ice bath conditions,Compounds 2-4 (30.0 g,150 mmol) was dissolved in N, N-dimethylformamide (300 mL)Sodium hydride (7.3 g, 300 mmol) was added slowlyTo the reaction system,Stirred at 0 C for 15 minutes;2,4,5-trichloropyrimidine (33.1 g, 180 mmol) was added dropwise to the reaction system,Room temperature reaction and stirring overnight;The reaction was completed, cooled and poured into 500 mL of water,Extracted with ethyl acetate, dried,Concentrated, silica gel column chromatography,To give compound 2-5 (17.3 g),Yield: 32.0%.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 5750-76-5.

Reference:
Patent; Hangzhou REX Pharmaceutical Co., Ltd; Wang, Yonghui; Gao, Yujun; Zhou, Juan; Zhu, Yan; Liu, Wandeng; Wang, Dong; Chen, Ximing; Wu, Yaodong; Li, Chunqi; (29 pag.)CN106336382; (2017); A;,
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. 302964-08-5, name is 2-((6-Chloro-2-methylpyrimidin-4-yl)amino)-N-(2-chloro-6-methylphenyl)thiazole-5-carboxamide, the common compound, a new synthetic route is introduced below. 302964-08-5

To a reaction flask, charged 2-((6-chloro-2-methylpyrimidin-4-yl)amino)-N-(2-chloro-6- methylphenyl)thiazole-5-carboxamide (20 g), N-(2-hydroxyl ethyl) piperazine (36 g) and n- butanol were added and the reaction mixture was refluxed for 3 hours to 4 hours. The resulting mixture was cooled and charged with phosphoric acid (10 g) and refluxed at a temperature of 50C to 60C. The reaction mixture was stirred for 1 hour at a temperature of 50C to 60C. The mixture obtained was then cooled to 25C to 35C and stirred for 1 hour maintaining the temperature. The resulting reaction mixture was then filtered and washed with methanol. To the reaction mixture charged water (400 mL) was added and further cooled at a temperature of 15C to 20C. Liquid ammonia (20 mL) was slowly added to the reaction mixture maintaining the temperature at 15C to 20C. The reaction mixture was stirred for 1 hour to isolate the product, amorphous dasatinib. The product was filtered, washed with water and dried under vacuum.

The synthetic route of 302964-08-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CIPLA LIMITED; COTTRILL, Emily; RAO, Dharmaraj Ramachandra; MALHOTRA, Geena; PATHI, Srinivas Laxminarayan; PUPPALA, Ravikumar; JAGANNADHAM, Yellanki; CHENNURU, Ramanaiah; (36 pag.)WO2018/78392; (2018); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia