HRID1513929

反应详情

EQUATION

反应方程式

HRID 1513929 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. extractionExtract with ethyl acetate (100 mL)
  2. customSeparate the layers
  3. washwash the organic layer with 10% aqueous lithium chloride solution (20 mL×2)
  4. dry with materialDry with magnesium sulfate
  5. concentrationconcentrate in vacuo
  6. customPurify the residue over silica gel
  7. washeluting the material with a step gradient of methanol/dichloromethane (0 to 10%)