反应 #1269897

反应方程式

Formylhydrazine

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

→

8-chloro-4H,6H-2,3,5,10b-tetraaza-benzo[e]azulene-5-carboxylic acid tert-butyl ester

收率 75.1%

溶剂

dioxane

反应条件

后处理

1. 1
   其他evaporated
2. 2
   其他The residue was purified by chromatography (300 g silica gel, heptane: ethyl acetate, 8:2 to 0:1)

实验过程

Formylhydrazine (10.7 g, 160 mmol) was added over a period of 4 hours to a solution of 7-chloro-2-thioxo-1,2,3,5-tetrahydro-benzo[e][1,4]diazepine-4-carboxylic acid tert-butyl ester (10.0 g, 32.0 mmol) in dioxane (200 ml) at 90° C. The reaction mixture was stirred at 90° C. overnight, then evaporated. The residue was purified by chromatography (300 g silica gel, heptane: ethyl acetate, 8:2 to 0:1) to yield 7.71 g (75%) 8-chloro-4H,6H-2,3,5,10b-tetraaza-benzo[e]azulene-5-carboxylic acid tert-butyl ester as white solid. MS m/e: 379 ([M+CH3COO−])

来源