反应详情

To a stirred solution of 0.10 g of 10,11-dihydro-10-(4-amino-3-methoxybenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine in 1 ml of methylene chloride is added 0.06 g of triethylamine followed by 0.05 g of iso-valeryl chloride. The reaction mixture is stirred for 3 hours and then quenched with 1N NaOH. The organic layer is evaporated in vacuo to a residue which is stirred in 5 ml of tetrahydrofuran for 1 hour, then evaporated in vacuo to a residue. The residue is extracted with ethyl acetate-methylene chloride, washed with brine, dried (Na2SO4), filtered through hydrous magnesium silicate and evaporated in vacuo to give 0.15 g of residue which is stirred with ether-hexane to give 0.13 g of light yellow solid. MS(CI): 418(M+H).

1. customquenched with 1N NaOH
2. customThe organic layer is evaporated in vacuo to a residue which
3. stirringis stirred in 5 ml of tetrahydrofuran for 1 hour
4. customevaporated in vacuo to a residue
5. extractionThe residue is extracted with ethyl acetate-methylene chloride
6. washwashed with brine
7. dry with materialdried (Na2SO4)
8. filtrationfiltered through hydrous magnesium silicate
9. customevaporated in vacuo