反应 #46394

反应方程式

5-amino-1,1-dioxo-2,3-dihydro-1H-1λ6-benzo[b]-thiophene-4-carboxylic acid

formamide

water

→

desired compound

收率 48.6%

3,3-dioxo-1,2,3,8-tetrahydro-3λ6-thia-6,8-diazacyclopenta-[a]naphthalen-9-one

收率 48.6%

溶剂

N,N-dimethyl-formamide

反应条件

后处理

1. 1
   其他reacted in a microwave at 150° C.
2. 2
   其他During the reaction
3. 3
   过滤The precipitated solid was filtered off with suction
4. 4
   洗涤washed successively with water and diethyl ether
5. 5
   其他dried in vacuo overnight

实验过程

0.87 g (3.83 mmol) of 5-amino-1,1-dioxo-2,3-dihydro-1H-1λ6-benzo[b]-thiophene-4-carboxylic acid was suspended in 2.0 ml of N,N-dimethyl-formamide and, after addition of 0.76 ml (19.14 mmol) of formamide, reacted in a microwave at 150° C. and 60 W for 40 min. During the reaction, the pressure in the microwave rose to 20 bar. The reaction mixture was then added to water. The precipitated solid was filtered off with suction and washed successively with water and diethyl ether and dried in vacuo overnight. 440 mg of the desired compound were obtained.

来源