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 2 ml of methylene chloride is added 60 mg of triethylamine followed by a solution of 56 mg of n-butylsulfonyl chloride in 0.5 ml of methylene chloride. After stirring at room temperature for 2 hours, the reaction mixture is evaporated in vacuo to a residue which is dissolved in methyl alcohol, stirred for 1hour and evaporated in vacuo to a residue which is treated with 2 ml of NH4Cl and extracted with 15 ml of ethyl acetate. The organic extract is washed with saturated NaHCO3, brine, dried (Na2SO4), filtered through hydrous magnesium silicate and the filtrate evaporated to a residue. The residue is stirred with ether-hexanes to give 0.14 g of light yellow solid. MS(CI): 454(M+H).

1. customthe reaction mixture is evaporated in vacuo to a residue which
2. dissolutionis dissolved in methyl alcohol
3. stirringstirred for 1hour
4. customevaporated in vacuo to a residue which
5. additionis treated with 2 ml of NH4Cl
6. extractionextracted with 15 ml of ethyl acetate
7. extractionThe organic extract
8. washis washed with saturated NaHCO3, brine
9. dry with materialdried (Na2SO4)
10. filtrationfiltered through hydrous magnesium silicate
11. customthe filtrate evaporated to a residue
12. stirringThe residue is stirred with ether-hexanes