反应 #159357

反应方程式

7-chloro-3,5-dihydrobenzo[e][1,4]oxazepin-2(1H)-one

2,4-bis-(4-methoxyphenyl)-1,3,2,4-dithiadiphosphetane-2,4-disulfide

→

title compound

收率 107.5%

7-Chloro-3,5-dihydrobenzo[e][1,4]oxazepine-2(1H)-thione

收率 107.5%

溶剂

tetrahydrofurane

反应条件

后处理

1. 1
   温度The reaction mixture was heated
2. 2
   温度at reflux for 4 h
3. 3
   其他was evaporated
4. 4
   其他the residue was crystallized from hot ethanol

实验过程

To a suspension of 7-chloro-3,5-dihydrobenzo[e][1,4]oxazepin-2(1H)-one (3.01 g, 15.2 mmol) in tetrahydrofurane (102 ml) was added 2,4-bis-(4-methoxyphenyl)-1,3,2,4-dithiadiphosphetane-2,4-disulfide (3.45 g, 8.53 mmol) at room temperature. The reaction mixture was heated at reflux for 4 h. After cooling to room temperature the solvent was evaporated and the residue was crystallized from hot ethanol to give the title compound (1.96 g, 60%) as light yellow solid. MS m/e: 211.6 ([M−H]−).

来源