تفاعل #546965

معادلة التفاعل

1-BOC-piperizine

2,6-dinitrobenzonitrile

water ethyl acetate

→

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

المردود 69.0%

المذيبات

DMF

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe reaction mixture was cooled to room temperature
2. 2
   غسيلThe organic fraction was washed with water and brine
3. 3
   تجفيفAfter drying over MgSO4
4. 4
   تركيزthe organic fraction was concentrated in vacuo
5. 5
   أخرىthe resulting brown residue was purified by flash chromatography

الإجراء التجريبي

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.

المصدر