反应 #302927

反应方程式

3-amino-4,5,6,7-tetrahydro-benzo[b]thiophene-2-carboxylic acid ethyl ester

chloroformamidine hydrochloride

→

desired compound

收率 95.5%

2-Amino-6,7,8,9-tetrahydro-1H-benzo[4,5]thieno[3,2-d]pyrimidin-4-one

收率 95.5%

溶剂

diethylene glycol dimethyl ether

反应条件

后处理

1. 1
   其他A 48 mL sealed tube
2. 2
   其他The tube was sealed
3. 3
   过滤Filtration

实验过程

A 48 mL sealed tube was charged with 3-amino-4,5,6,7-tetrahydro-benzo[b]thiophene-2-carboxylic acid ethyl ester (2.8 g, 12.3 mmol), chloroformamidine hydrochloride (2.0 g, 17.2 mmol), and diethylene glycol dimethyl ether (24.6 mL). The tube was sealed and heated to 160° C. for 12 h with vigorous stirring. Filtration afforded the desired compound as a beige solid (2.6 g). MS: No signal. 1H NMR (400 MHz, d6-DMSO) δ ppm 2.84-2.73 (m, 2H), 2.58-2.51 (m, 2H), 1.89-1.70 (m, 4H).

来源