反应详情

To a suspension of Example 180E (17.7 g, 46.4 mmol) in 200 mL of ethanol/water (4:1) at 0° C. was added NaBH4 (8.9 g, 0.232 mol) portion-wise. After stirring for 0.5 hour, the mixture was quenched with 1N HCl to pH 4-5 and concentrated under reduced pressure. The residue was dissolved in 100 mL of saturated aqueous K2CO3 and extracted with dichloromethane. The organic phase was washed with brine, dried and purified by column chromatography on silica gel eluting with dichloromethane/methanol (30:1) to obtain the title compound.

1. customthe mixture was quenched with 1N HCl to pH 4-5
2. concentrationconcentrated under reduced pressure
3. dissolutionThe residue was dissolved in 100 mL of saturated aqueous K2CO3
4. extractionextracted with dichloromethane
5. washThe organic phase was washed with brine
6. customdried
7. custompurified by column chromatography on silica gel eluting with dichloromethane/methanol (30:1)