反応 #4906

反応方程式

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

phosphorus pentasulfide

potassium sulfide

→

product

収率 86.1%

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

収率 86.1%

溶媒

toluene

反応条件

後処理

1. 1
   ろ過The reaction mixture was filtered
2. 2
   濃縮the filtrate concentrated under reduced pressure
3. 3
   その他to give a yellow solid
4. 4
   その他Recrystallization from absolute ethanol

実験手順

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.

出典