反应详情

To a solution of the crude compound from Example 10 (76 mmol) in methanol (170 mL) is added sodium borohydride (1.93 g, 51 mmol) portion-wise and the reaction stirred for 3 hr. The reaction is quenched with ice-water (50 mL) and the methanol is removed under reduced pressure on a rotary evaporator. The residual aqueous phase is extracted with ethyl acetate (2×100 mL) to yield crude product (25 g). This crude product is purified by column chromatography on silica gel eluted with ethyl acetate/hexane to yield the title compound (1.8 g, 8.6%). MS m/z 409.1 (M+.+1).

1. customThe reaction is quenched with ice-water (50 mL)
2. customthe methanol is removed under reduced pressure on a rotary evaporator
3. extractionThe residual aqueous phase is extracted with ethyl acetate (2×100 mL)
4. customto yield crude product (25 g)
5. customThis crude product is purified by column chromatography on silica gel
6. washeluted with ethyl acetate/hexane