HRID1595227
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution the product of step 2 (500 mg) in DMF (20 ml) were added 4-(4-chlorophenyl)-4-hydroxypiperidine (50 mg), potassium carbonate (430 mg), potasium iodide (130 mg) and the mixture was stirred at room temperature for 12 hours. Water and ethyl acetate were added to the reaction mixture, the organic layer was separated and washed with saturated aqueous sodium chloride, and dried with magnesium sulfate. The solvent was distilled off under reduced pressure. The residue was purified by silica gel chromatography eluting with methylene chloride-methanol (10:1) to give the titled compound as major regioisomer (225 mg) and minor one (140 mg).
WORKUP
后处理
- customthe organic layer was separated
- washwashed with saturated aqueous sodium chloride
- dry with materialdried with magnesium sulfate
- distillationThe solvent was distilled off under reduced pressure
- customThe residue was purified by silica gel chromatography
- washeluting with methylene chloride-methanol (10:1)