反应详情

To a solution of 92 mg of 10, 11-dihydro-5H-pyrrolo[2, 1-c][1,4]benzodiazepine in 2 ml of methylene chloride is added 100 mg of triethylamine followed by 130 mg of 4-(n-butyloxy)benzoyl chloride. The reaction mixture is stirred am room temperature for 24 hours and then treated with 4 ml of in sodium hydroxide. The mixture is extracted with 10 ml of ethyl acetate and the extract washed with 1N sodium hydroxide and 5 ml of brine. The organic layer is dried over anhydrous sodium sulfate and filtered through hydrous magnesium silicate. The filtrate is concentrate in vacuo to a residue which is stirred with ether-hexanes to give 160 mg of the desired product as a white solid:mass spectrum (CI), 361(MH+).

1. extractionThe mixture is extracted with 10 ml of ethyl acetate
2. washthe extract washed with 1N sodium hydroxide and 5 ml of brine
3. dry with materialThe organic layer is dried over anhydrous sodium sulfate
4. filtrationfiltered through hydrous magnesium silicate
5. concentrationThe filtrate is concentrate in vacuo to a residue which
6. stirringis stirred with ether-hexanes