HRID2119326

反应详情

EQUATION

反应方程式

HRID 2119326 的结构方程式

PROCEDURE

实验过程

A mixture of N-benzylmethylamine (3.6 g, 30 mmol) and 4-(3-fluoro-4-nitrobenzyl)morpholine (2.4 g, 10 mmol) in acetonitrile (3.0 mL) is heated under reflux for 30 min and the solvent is then removed under reduced pressure. The residual oil is partitioned between ethyl acetate (70 mL) and sodium hydroxide solution (10 mL of 1 N) and the ethyl acetate phase is separated and washed twice with water (5 mL). The ethyl acetate is removed and the crude product is applied to a silica gel column. The column is eluted with 50% ethyl acetate/hexane to give 3.3 g of the title compound as an oil.

WORKUP

后处理

  1. temperatureis heated
  2. temperatureunder reflux for 30 min
  3. customthe solvent is then removed under reduced pressure
  4. customThe residual oil is partitioned between ethyl acetate (70 mL) and sodium hydroxide solution (10 mL of 1 N)
  5. customthe ethyl acetate phase is separated
  6. washwashed twice with water (5 mL)
  7. customThe ethyl acetate is removed
  8. washThe column is eluted with 50% ethyl acetate/hexane