反应 #302920

反应方程式

ethyl chloroformate

3-amino-thiophene-2-carboxylic acid methyl ester

K2CO3

→

desired product

收率 98.4%

3-Ethoxycarbonylamino-thiophene-2-carboxylic acid methyl ester

收率 98.4%

溶剂

benzene

反应条件

后处理

1. 1
   温度After heating
2. 2
   温度at reflux for 12 h
3. 3
   过滤the mixture was filtered
4. 4
   浓缩the filtrate was concentrated

实验过程

To a solution of 3-amino-thiophene-2-carboxylic acid methyl ester (2.39 g, 15.2 mmol) in benzene (51 mL) was added K2CO3 (6.30 g, 45.6 mmol) followed by ethyl chloroformate (1.74 mL, 18.2 mmol). After heating at reflux for 12 h, the mixture was filtered and the filtrate was concentrated to afford the desired product (3.43 g), which was used in the next step without further purification. MS: 230.0. 1H NMR (400 MHz, CD3OD) δ ppm 7.82 (d, J=5.5 Hz, 1H), 7.66 (d, J=5.6 Hz, 1H), 4.23 (q, J=7.1 Hz, 2H), 3.86 (s, 3H), 1.32 (t, J=7.1 Hz, 3H).

来源