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ChemicalBook CAS DataBase List 4-Chloro-2-methyl-1H-pyrrolo[2,3-d]pyrimidine

4-Chloro-2-methyl-1H-pyrrolo[2,3-d]pyrimidine synthesis

3synthesis methods
-

Yield: 95.8%

Reaction Conditions:

with tetraethylammonium chloride;trichlorophosphate at 60 - 80; for 0.5 h;

Steps:

6 Example 6: Preparation of 2-methyl-4-chloropyrrolopyrimidine.
A 2L three-necked flask is equipped with a thermometer and a condenser,Add 184g of phosphorus oxychloride, 16.6g of tetraethylammonium chloride, and warm up to 60 ,Add 149g of 2-methyl-4-hydroxypyrrolopyrimidine in portions and warm to 80 ° C,Incubate the reaction for 30 minutes, HPLC traces the reaction of the raw materials to completion, and lower the temperature to 30 ° C.Prepare 2 liters of 10% sodium hydroxide solution, slowly add the reaction solution to extract,Precipitate solid, filter by suction to get semi-finished product, recrystallize ethyl ester,The finished product was 161g after drying, and the yield was 95.8%.

References:

Anqing Bo Man Biological Co., Ltd.;Chen Jia;He Xueyin;Liu Pengcheng CN110950806, 2020, A Location in patent:Paragraph 0031-0034

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