HRID1032328

反应详情

EQUATION

反应方程式

HRID 1032328 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Alpha-bromo-1,2-benzisoxazole-3-acetic acid (58.0 g, 0.23 mole) is suspended in toluene (350 mL) and the mixture is stirred at reflux for 18 hours. The solvent is evaporated and the residue is taken up in methylene chloride (250 mL). This solution is washed with saturated aqueous sodium bicarbonate (2×50 mL), water (50 mL) and dried over anhydrous magnesium sulfate. The solution is filtered and evaporated to afford 3-bromomethyl-1,2-benzisoxazole, m.p. 60-62° C. The compound is purified by recrystallisation from ether-hexane, m.p. 64-66° C.

WORKUP

后处理

  1. temperatureat reflux for 18 hours
  2. customThe solvent is evaporated
  3. washThis solution is washed with saturated aqueous sodium bicarbonate (2×50 mL), water (50 mL)
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationThe solution is filtered
  6. customevaporated