反应 #4906

反应方程式

7-chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepin-5(4H)-one

phosphorus pentasulfide

potassium sulfide

→

product

收率 86.1%

7-Chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepine-5(4H)-thione

收率 86.1%

溶剂

toluene

反应条件

后处理

1. 1
   过滤The reaction mixture was filtered
2. 2
   浓缩the filtrate concentrated under reduced pressure
3. 3
   其他to give a yellow solid
4. 4
   其他Recrystallization from absolute ethanol

实验过程

To a solution of 20 g (0.07 mole) of 7-chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepin-5(4H)-one in 200 ml of toluene was added a mixture of 9.55 g (0.05 mole) of phosphorus pentasulfide and 9.5 g of potassium sulfide which had been ground together. The reaction mixture was filtered and the filtrate concentrated under reduced pressure to give a yellow solid. Recrystallization from absolute ethanol gave 12.5 g (68%) of the product, m.p. 102°-104° C.

来源