HRID1623659

反应详情

EQUATION

反应方程式

HRID 1623659 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of methyl 2,5-dihydroxybenzoate (10 g, 59.5 mmol), potassium carbonate (50.0 g, 362 mmol), and dry acetone (450 ml) was stirred at room temperature for 30 min. 4-Methylbenzenesulfonyl chloride (11.44 g, 60.0 mmol) was added portionwise and the mixture was refluxed for 7 h. (Bromomethyl)benzene (25.4 g, 149 mmol) was added and the resulting mixture was refluxed overnight. After cooling, the precipitate was filtered, and the filtrate was evaporated. The residue was loaded onto a silica gel column and was eluted with hexane/ethyl acetate=4:1 to yield the title compound as a yellow solid. 22 g.

WORKUP

后处理

  1. additionwas added
  2. temperaturethe resulting mixture was refluxed overnight
  3. temperatureAfter cooling
  4. filtrationthe precipitate was filtered
  5. customthe filtrate was evaporated
  6. washwas eluted with hexane/ethyl acetate=4:1