反应 #1269896

反应方程式

7-chloro-2-oxo-1,2,3,5-tetrahydro-benzo[1,4]diazepine-4-carboxylic acid tert-butyl ester

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

→

title compound

收率 157.1%

7-Chloro-2-thioxo-1,2,3,5-tetrahydro-benzo[e][1,4]diazepine-4-carboxylic acid tert-butyl ester

收率 157.1%

溶剂

tetrahydrofuran

反应条件

后处理

1. 1
   温度was heated
2. 2
   温度at reflux for 3 h
3. 3
   其他The solvent was evaporated
4. 4
   其他the residue was triturated in tort-butyl methyl ether
5. 5
   其他The precipitate was removed by filtration
6. 6
   浓缩the filtrate was concentrated to dryness
7. 7
   其他The residue was crystallized from hot ethanol

实验过程

A mixture of 7-chloro-2-oxo-1,2,3,5-tetrahydro-benzo[1,4]diazepine-4-carboxylic acid tert-butyl ester (41.1 g, 0.139 mol) and 2,4-bis-(4-methoxyphenyl)-1,3,2,4-dithiadiphosphetane-2,4-disulfide (31.5 g, 0.0763 mol) in tetrahydrofuran (1100 ml) was heated at reflux for 3 h. The solvent was evaporated and the residue was triturated in tort-butyl methyl ether. The precipitate was removed by filtration and the filtrate was concentrated to dryness. The residue was crystallized from hot ethanol to give the title compound (37.5 g, 86.4%) as light yellow solid. MS m/e: 311 (M−H+).

来源