반응 #546965

반응 방정식

1-BOC-piperizine

2,6-dinitrobenzonitrile

water ethyl acetate

→

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

수율 69.0%

용매

DMF

반응 조건

후처리

1. 1
   온도the reaction mixture was cooled to room temperature
2. 2
   세척The organic fraction was washed with water and brine
3. 3
   건조After drying over MgSO4
4. 4
   농축the organic fraction was concentrated in vacuo
5. 5
   기타the resulting brown residue was purified by flash chromatography

실험 절차

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.

출처