HRID527538

反应详情

EQUATION

反应方程式

HRID 527538 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3-(methyloxy)phenol (10.38 g, 84 mmol) in tetrahydrofurane (100 ml, SCRC) was added NaH (60% wt., 1.824 g, 76 mmol, Aldrich) portionwise under ice-cooling. The reaction mixture was stirred at room temperature for 1 hour and bromomethyl methyl ether (9.5 g, 76 mmol, SCRC) was then added. The resulting mixture was stirred at room temperature for 2 hours and water (50 ml) was added. The reaction mixture was extracted with ethyl acetate (2 times 50 ml, SCRC) and the combined organic layers were dried over sodium sulphate, evaporated. The residue was purified by column chromatography on silica gel (EtOAc:PE=1:100) to afford the title compound (10.2 g) as a colorless liquid.

WORKUP

后处理

  1. temperaturecooling
  2. stirringThe resulting mixture was stirred at room temperature for 2 hours
  3. extractionThe reaction mixture was extracted with ethyl acetate (2 times 50 ml, SCRC)
  4. dry with materialthe combined organic layers were dried over sodium sulphate
  5. customevaporated
  6. customThe residue was purified by column chromatography on silica gel (EtOAc:PE=1:100)