反应详情

To a stirred solution of the product from Method A (38 grams/0.171 mol) dissolved in 140 mL of 10:1 ethanol/water at 0° C. was added 16 grams (0.427 mol) of sodium borohydride portion-wise over 25 minutes. The resulting mixture stirred for 18 hours at room temperature, at which time, the reaction was quenched upon addition of 100 mL of water. The reaction mixture was filtered, the filter cake washed with water and ethylacetate, and the combined filtrates concentrated under reduced pressure to remove the organics. The residue was diluted with water (100 mL) and extracted 3 times with 150 mL with ethylacetate. The combined ethylacetate extracts were dried over Na2SO4 and concentrated to dryness in vacuo affording 32 grams (100%) of the title compound as a yellow oil. LRMS: 188 (M+1).

1. customthe reaction was quenched upon addition of 100 mL of water
2. filtrationThe reaction mixture was filtered
3. washthe filter cake washed with water and ethylacetate
4. concentrationthe combined filtrates concentrated under reduced pressure
5. customto remove the organics
6. additionThe residue was diluted with water (100 mL)
7. extractionextracted 3 times with 150 mL with ethylacetate
8. dry with materialThe combined ethylacetate extracts were dried over Na2SO4
9. concentrationconcentrated to dryness in vacuo