HRID1532992

反应详情

EQUATION

反应方程式

HRID 1532992 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The crude 2-[(2-methoxyphenoxy)methyl]morpholine (2.0 g, 9.0 mmol) was mixed with 4-trifluoromethylbenzylbromide (2.58 g, 10.8 mmol), potassium carbonate (6.84 g, 49.5 mmol) in ethanol (50 ml) and refluxed for 3.5 h. Water was added and the product was extracted with 2 portions of ethyl acetate. Drying and evaporation gave the crude free base. Dissolution in ether and precipitation with oxalic acid gave a salt that was purified by recrystallization from ethanol and then THF. Yield 430 mg, 10%, mp 101-108° C.

WORKUP

后处理

  1. temperaturerefluxed for 3.5 h
  2. extractionthe product was extracted with 2 portions of ethyl acetate
  3. customDrying
  4. customevaporation
  5. customgave the crude free base
  6. customprecipitation with oxalic acid
  7. customgave a salt that
  8. customwas purified by recrystallization from ethanol