反应详情

To a solution of 10 mmol of 9,10-dihydro-4H-pyrrolo[1,2-a]thieno[2,3-e][1,4]diazepine in 50 ml of methylene chloride under argon is added 15 mmol of triethylamine followed by ice bath cooling. A solution of 11 mmol of 4-nitrobenzoyl chloride in 10 ml of methylene chloride is added dropwise. Following complete addition, the ice bat]h 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, 1N HCl, NaCHO3, and brine. The organic layer is dried with Na2SO4, filtered and evaporated in vacuo to give a solid which is purified by flash chromatography on silica gel to give desired product as a solid.

1. customfollowed by ice bath
2. temperaturecooling
3. additionaddition
4. customthe ice bat]h is removed
5. customThe volatiles are removed in vacuo
6. customto give a residue which
7. washThe solution is washed with water, 1N HCl, NaCHO3, 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 on silica gel