反应详情

The product from Example 1, Step A (8.87 g, 20.2 mmol) was dissolved in methanol (50 mL) and methylene chloride (20 mL). Sodium borohydride (764 mg, 20.2 mmol) was added in portions at 0° C., and the solution was stirred for 2 hours. The reaction was quenched by the addition of saturated aqueous ammonium chloride until hydrogen evolution ceased. The resulting suspension was concentrated in vacuo and then partitioned between methylene chloride (50 mL) and saturated aqueous sodium bicarbonate (50 mL). The layers were separated and the aqueous layer was extracted with methylene chloride (3×100 mL). The combined organic layers were dried over sodium sulfate, filtered, and concentrated in vacuo to provide the title product as a yellow oil which was sufficiently pure for use in the next step.

1. customThe reaction was quenched by the addition of saturated aqueous ammonium chloride until hydrogen evolution
2. concentrationThe resulting suspension was concentrated in vacuo
3. custompartitioned between methylene chloride (50 mL) and saturated aqueous sodium bicarbonate (50 mL)
4. customThe layers were separated
5. extractionthe aqueous layer was extracted with methylene chloride (3×100 mL)
6. dry with materialThe combined organic layers were dried over sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated in vacuo