反应 #546965

反应方程式

1-BOC-piperizine

2,6-dinitrobenzonitrile

water ethyl acetate

→

4-(2-cyano-3-nitro-phenyl)-piperazine-1-carboxylic acid tert-butyl ester

收率 69.0%

溶剂

DMF

反应条件

后处理

1. 1
   温度the reaction mixture was cooled to room temperature
2. 2
   洗涤The organic fraction was washed with water and brine
3. 3
   干燥After drying over MgSO4
4. 4
   浓缩the organic fraction was concentrated in vacuo
5. 5
   其他the resulting brown residue was purified by flash chromatography

实验过程

1-BOC-piperizine (piperazine-1-carboxylic acid tert-butyl ester, 20.0 g, 107.4 mmol) was added to a solution of 2,6-dinitrobenzonitrile (10.277 g, 53.2 mmol) in dry DMF (200 ml). After stirring at 50° C. overnight, the reaction mixture was cooled to room temperature and poured into a mixture of water/ethyl acetate. The organic fraction was washed with water and brine. After drying over MgSO4, the organic fraction was concentrated in vacuo and the resulting brown residue was purified by flash chromatography to give 4-(2-cyano-3-nitro-phenyl)-piperazine-1-carboxylic acid tert-butyl ester as an orange solid (12.172 g, 69%). MS: (M+H)+277.1.

来源