HRID1026353

反应详情

EQUATION

反应方程式

HRID 1026353 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a mixture of 2-(2-bromo-4-(methoxymethoxy)phenyl)-N-methoxy-N-methylacetamide (4.30 g) in ether (93 ml) was added methyl magnesium bromide (3 M in ether, 63 mL) dropwise at 0° C. After addition, the solution was stirred at 0° C. for 1.5 hr. The mixture was poured into saturated aqueous ammonium chloride, and extracted with ethyl acetate (100 mL×2). The organic phase was dried over anhydrous sodium sulfate, The solvent was removed under reduced pressure, and the residue was purified by silica gel column chromatography (petroleum ether/ethyl acetate) to afford the title compound (23 g).

WORKUP

后处理

  1. additionAfter addition
  2. extractionextracted with ethyl acetate (100 mL×2)
  3. dry with materialThe organic phase was dried over anhydrous sodium sulfate
  4. customThe solvent was removed under reduced pressure
  5. customthe residue was purified by silica gel column chromatography (petroleum ether/ethyl acetate)