HRID1861971
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
PROCEDURE
实验过程
To a mixture of the compound (100 mg) obtained in Example 565, nickel (II) chloride hexahydrate (123 mg) and methanol (6 ml), sodium borohydride (39 mg) was added. The reaction mixture was stirred at room temperature for 10 min; then, 2 N HCl was added and a saturated aqueous sodium bicarbonate solution and chloroform were also added. The organic layer was washed with a saturated aqueous sodium chloride solution, dried with anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent, n-hexane:ethyl acetate=3:2) to give 87 mg of the titled compound (yield, 94%).
WORKUP
后处理
- additionwas added
- washThe organic layer was washed with a saturated aqueous sodium chloride solution
- dry with materialdried with anhydrous sodium sulfate
- distillationthe solvent was distilled off under reduced pressure
- customThe resulting residue was purified by silica gel column chromatography (eluent, n-hexane:ethyl acetate=3:2)