反应 #4907

反应方程式

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

phosphorus pentasulfide

potassium sulfide

→

product

收率 86.3%

2-(2-Chloroethyl)-2,3-dihydro-7-methoxy-4-methyl-1,4-benzoxazepine-5(4H)-thione

收率 86.3%

溶剂

chloroform

反应条件

后处理

1. 1
   温度heated
2. 2
   温度at reflux under nitrogen atmosphere for 5 hr
3. 3
   过滤The mixture was filtered hot
4. 4
   浓缩the filtrate concentrated under reduced pressure
5. 5
   其他The residue, an orange solid, was recrystallized from ethanol

实验过程

To a solution of 10.3 g (0.04 mole) of 2-(2-chloroethyl)-2,3-dihydro-7-methoxy-4-methyl-1,4-benzoxazepin-5(4H)-one in 200 ml of chloroform was added a mixture of 5.7 g (0.03 mole) of phosphorus pentasulfide and 5.7 g of potassium sulfide which had been ground together. The reaction mixture was stirred and heated at reflux under nitrogen atmosphere for 5 hr. The mixture was filtered hot and the filtrate concentrated under reduced pressure. The residue, an orange solid, was recrystallized from ethanol to give 7.4 g (65%) of product, m.p. 98°-100° C.

来源