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 1 hour 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 1 hour
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