HRID270044

反应详情

EQUATION

反应方程式

HRID 270044 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Sodium hydride (350 mg, 7.0 mmol, 50% disp in oil) was washed three times with heptane, under nitrogen atmosphere, and then dissolved in tetrahydrofuran (50 mL). A solution of [1-benzyl-4-(2-fluorobenzyl)piperidin-4-yl)methanol (1 g, 3.2 mmol) in tetrahydrofuran (30 mL) was added and the resulting mixture was refluxed for 3 hrs. The cooled solution was partitioned between water and ethyl acetate and the organic layer was dried over magnesium sulphate and concentrated. The crude product was purified on silica (dichloromethane/methanol) to give 0.83 g (89%) of the subtitle compound.

WORKUP

后处理

  1. temperaturethe resulting mixture was refluxed for 3 hrs
  2. customThe cooled solution was partitioned between water and ethyl acetate
  3. dry with materialthe organic layer was dried over magnesium sulphate
  4. concentrationconcentrated
  5. customThe crude product was purified on silica (dichloromethane/methanol)