Analyzing the synthesis route of 137281-39-1

Statistics shows that 137281-39-1 is playing an increasingly important role. we look forward to future research findings about 4-(2-(2-Amino-4-oxo-4,7-dihydro-1H-pyrrolo[2,3-d]pyrimidin-5-yl)ethyl)benzoic acid.

137281-39-1, 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. 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, the common compound, a new synthetic route is introduced below.

4- [2- (2-amino-4,7-dihydro-4-oxo-3H-pyrrolo [2,3-d] pyrimidin-5-yl) ethyl] benzoic acid (64.6 g 0.19 mol) Add 1L four-necked flask, add 650ml DMF, stir to dissolve, warm to 50 C, add 0.38molN, N-carbonyldiimidazole, and incubate at 60 C for 2 hours, add L-glutamic acid diethyl ester (0.38mol), and warm to Reaction at 80 C for 3 hours, evaporated to dryness under reduced pressure, added 800ml of dichloromethane to dissolve, poured into a mixed solution of 1600ml pure water and 160ml triethylamine, stirred and separated, separated the organic phase, washed twice with pure water 1600ml ¡Á 2 Dry, evaporate to dryness, add 500ml of absolute ethanol and stir to dissolve. Add 72g of p-toluenesulfonic acid monohydrate and 200ml of absolute ethanol solution dropwise under reflux. After the addition is complete, reflux for 1 hour, cool down and crystallize, suction filter, and dry. 87.2 g of crude product was obtained (molar yield 70.1%, purity 92.3%, impurity V content was 6.52%).Add 87.2g of the above crude product to a three-necked reaction flask, add 350ml of N, N-dimethylformamide, heat to 40-45 C, stir to dissolve, add 700ml of absolute ethanol dropwise after complete dissolution, and slowly precipitate a solid. The temperature was lowered to room temperature, and the mixture was crystallized by stirring for 1-2 hours. The solid was filtered to obtain 69.8 g, and the yield was 80.0%.The above-mentioned refining operation was repeated once to obtain 55.4 g of a solid (purity: 98.2%, impurity V content: 0.07%).

Statistics shows that 137281-39-1 is playing an increasingly important role. we look forward to future research findings about 4-(2-(2-Amino-4-oxo-4,7-dihydro-1H-pyrrolo[2,3-d]pyrimidin-5-yl)ethyl)benzoic acid.

Reference:
Patent; Lunan Pharmaceutical Group Co., Ltd.; Zang Chao; (10 pag.)CN110305134; (2019); A;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia