HRID1532992
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
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
- temperaturerefluxed for 3.5 h
- extractionthe product was extracted with 2 portions of ethyl acetate
- customDrying
- customevaporation
- customgave the crude free base
- customprecipitation with oxalic acid
- customgave a salt that
- customwas purified by recrystallization from ethanol