HRID633555
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 50 °C
PROCEDURE
实验过程
The product from Example 60A (1.0 g, 3.03 mmol) and borane tetrahydrofuran complex (6.06 mL, 6.06 mmol) were combined in tetrahydrofuran (15.15 mL) and heated at 50° C. for 2 hours, cooled, treated with 10 mL of methanol, heated at 50° C. for 1 hour, cooled and concentrated. The residue was partitioned between ethyl acetate and water. The organic layer was washed with saturated aqueous sodium chloride, dried (anhydrous Na2SO4), filtered, and concentrated. Purification by chromatography (silica gel, 0-50% ethyl acetate in heptanes) afforded the title compound (0.73 g, 76%).
WORKUP
后处理
- temperaturecooled
- temperatureheated at 50° C. for 1 hour
- temperaturecooled
- concentrationconcentrated
- customThe residue was partitioned between ethyl acetate and water
- washThe organic layer was washed with saturated aqueous sodium chloride
- dry with materialdried (anhydrous Na2SO4)
- filtrationfiltered
- concentrationconcentrated
- customPurification by chromatography (silica gel, 0-50% ethyl acetate in heptanes)