反应详情

To a solution of 10 mmol of 10,11-dihydro-5H-imidazo[2,1-c][1,4]benzodiazepine in 50 ml of methylene chloride under argon is added 15 mmol of triethylamine followed by ice bath cooling. A solution of 10 mmol of 4-nitrobenzoyl chloride in 10 ml of methylene chloride is added dropwise. Following complete addition, the ice bath is removed and the reaction mixture stirred at room temperature for 2 hours. The volatiles are removed in vacuo to give a residue which is dissolved in ethyl acetate. The solution is washed with water, and brine. The organic layer is dried with Na2SO4, filtered and evaporated in vacuo to give a solid which is purified by flash chromatography to give desired product as a solid.

1. customfollowed by ice bath
2. temperaturecooling
3. additionaddition
4. customthe ice bath is removed
5. customThe volatiles are removed in vacuo
6. customto give a residue which
7. washThe solution is washed with water, and brine
8. dry with materialThe organic layer is dried with Na2SO4
9. filtrationfiltered
10. customevaporated in vacuo
11. customto give a solid which
12. customis purified by flash chromatography