反应详情

To a solution of 500 mg of the compound obtained in Step 198-3 in CHCl3 (3.5 ml) was added piperidine (0.14 ml) and acetic acid (0.24 ml), and the reaction mixture was stirred for 30 minutes. To the solution was added 327 mg of sodium triacetoxy borohydride, and the reaction mixture was further stirred for 15 hours. After the end of the reaction, water was added to the solution and the resulting mixture was extracted with CHCl3. The organic layer was washed with saturated brine and dried over MgSO4, then, the drying agent was separated by filtration and the solvent was evaporated under reduced pressure. The obtained residue was purified by column chromatography (silicagel 60; mobile phase: MeOH/CHCl3=1/99; v/v) to obtain respectively 94 mg (Isomer A: colorless amorphous) and 217 mg (Isomer B: colorless amorphous) of two species of diastereoisomers of the title compound.

1. stirringthe reaction mixture was further stirred for 15 hours
2. additionwas added to the solution
3. extractionthe resulting mixture was extracted with CHCl3
4. washThe organic layer was washed with saturated brine
5. dry with materialdried over MgSO4
6. customthe drying agent was separated by filtration
7. customthe solvent was evaporated under reduced pressure
8. customThe obtained residue was purified by column chromatography (silicagel 60; mobile phase: MeOH/CHCl3=1/99; v/v)