HRID1532851

反应详情

EQUATION

反应方程式

HRID 1532851 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension in DMF (3.5 mL) of sodium hydride (60% in mineral oil, 52 mg, 1.3 mmol) was added 2-thiophenemethanol (0.135 mL, 1.4 mmol) and the reaction mixture was stirred for 1.25 hours. 4-bromomethyl-2-(2-methylphenyl)benzoic acid methyl ester (0.35 mL, 1.2 mmol) was added and the reaction mixture was stirred for 2 hours. The reaction mixture was partitioned between water and ether. The aqueous phase was extracted with ether. The combined organic layers were washed with brine, dried over sodium sulfate, filtered and concentrated in vacuo. Chromatography on silica gel (3% ethyl acetate-hexane) gave 4-(2-thienylmethoxymethyl)-2-(2-methylphenyl)benzoic acid methyl ester (250 mg).

WORKUP

后处理

  1. stirringthe reaction mixture was stirred for 2 hours
  2. customThe reaction mixture was partitioned between water and ether
  3. extractionThe aqueous phase was extracted with ether
  4. washThe combined organic layers were washed with brine
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo