HRID1513929
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
Alternatively, dissolve enantiomerically enriched 5-{hydroxy-[4-(2-piperidin-1-yl-ethoxy)-phenyl]-methyl}-6-(2,4,6-trifluoro-phenyl)-naphthalen-2-ol (804 mg, 1.59 mmol) in DMF (10 mL). Add potassium tert-butoxide (532 mg, 4.75 mmol). Heat at 50° C. for 2 minutes. Pour the reaction mixture into ice (5 g). Extract with ethyl acetate (100 mL). Separate the layers and wash the organic layer with 10% aqueous lithium chloride solution (20 mL×2). Dry with magnesium sulfate and concentrate in vacuo. Purify the residue over silica gel, eluting the material with a step gradient of methanol/dichloromethane (0 to 10%), to give the enantiomerically enriched title compound.
WORKUP
后处理
- extractionExtract with ethyl acetate (100 mL)
- customSeparate the layers
- washwash the organic layer with 10% aqueous lithium chloride solution (20 mL×2)
- dry with materialDry with magnesium sulfate
- concentrationconcentrate in vacuo
- customPurify the residue over silica gel
- washeluting the material with a step gradient of methanol/dichloromethane (0 to 10%)