反应 #675928

反应方程式

ammonia

ethyl 2-amino-4-methylthiophene-3-carboxylate

chloroformamidine hydrochloride

dimethylsulfone

→

title compound

收率 87.9%

2-Amino-5-methylthieno[2,3-d]pyrimidin-4(1H)-one

收率 87.9%

溶剂

Water

反应条件

后处理

1. 1
   温度the mixture was cooled down to room temperature
2. 2
   过滤The precipitate was filtered off

实验过程

A mixture of ethyl 2-amino-4-methylthiophene-3-carboxylate (2.0 g, 11.7 mmol), chloroformamidine hydrochloride (3.357 g, 29.0 mmol) and dimethylsulfone (5.489 g, 58.4 mmol) was heated at 135° C. for 45 minutes. Water was added and the mixture was cooled down to room temperature. An aqueous ammonia solution was added to adjust the solution to pH 9. The precipitate was filtered off, yielding the title compound (1.863 g) as a white powder. 13C NMR δ (75 MHz, DMSO-d6) 168.98, 159.12, 153.21, 133.26, 114.37, 110.81, 16.35. MS (m/z) 182 [M+H]+.

来源