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温度

0 °C

To a suspension of 11 (700 mg, 2.88 mmol) in methanol (15 mL) at 0° C. was added sodium borohydride (164 mg, 4.32 mmol) and the resulting reaction mixture was allowed to stir at 0° C. for 2 hours. The reaction mixture was concentrated in vacuo to remove methanol and the residue was taken up in ethyl acetate and poured onto 1N HCl and extracted with ethyl acetate (3×30 mL). The combined ethyl acetate extracts were dried over anhydrous sodium sulfate and concentrated in vacuo to provide 612 mg of 12 as a yellow solid (706 mg theoretical, 87% yield).

1. customthe resulting reaction mixture
2. concentrationThe reaction mixture was concentrated in vacuo
3. customto remove methanol
4. additionpoured onto 1N HCl
5. extractionextracted with ethyl acetate (3×30 mL)
6. dry with materialThe combined ethyl acetate extracts were dried over anhydrous sodium sulfate
7. concentrationconcentrated in vacuo