反应详情

7-[(1-[2(R)-((1,1-dimethylethoxy)carbonyl)amino-4-methylpentanoyl]-2,3-dihydro-1H-indol-3-yl)methyl]quinazolino(3,2-A)-1,4-benzodiazepin-5,13-(6H,7H)-dione (120 mg, 0.19 mmole) was dissolved in 3 ml of glacial acetic acid and treated at 10° with 48 mg (0.77 mmole) of sodium cyanoborohydride. After twenty minutes, the reaction mixture was poured into 50 ml of water, extracted with ethyl acetate (4×40 ml) and the combined organic extracts were washed with saturated sodium bicarbonate solution and brine, then dried (MgSO4) and concentrated. The crude product was purified by preparative thick layer chromatography on silica gel (98:2 chloroform-methanol, multiple elutions) to give the analytical product as isomer 2, the slower eluting component.

1. waitAfter twenty minutes
2. extractionextracted with ethyl acetate (4×40 ml)
3. washthe combined organic extracts were washed with saturated sodium bicarbonate solution and brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated
6. customThe crude product was purified by preparative thick layer chromatography on silica gel (98:2 chloroform-methanol, multiple elutions)
7. customto give the analytical product as isomer 2
8. washthe slower eluting component