HRID1065244

反应详情

EQUATION

反应方程式

HRID 1065244 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The solution of 48.6 g of 2-(7-methyl-1,4-benzodioxan-2-yl)-acetic acid in the minimum amount of tetrahydrofuran is added dropwise at reflux rate to the stirred suspension of 13.4 g of lithium aluminum hydride in 200 ml of dry tetrahydrofuran. The mixture is refluxed overnight, cooled, and decomposed by the addition of 13.4 ml of water, 13.4 ml 15% aqueous sodium hydroxide and 40 ml of water. It is filtered, evaporated, the residue distilled in a molecular still, and the fraction boiling at 155°-165°/0.1 mmHg collected as colorless oil, to yield the 2-(2-hydroxyethyl)-7-methyl-1,4-benzodioxan.

WORKUP

后处理

  1. temperatureat reflux rate
  2. temperatureThe mixture is refluxed overnight
  3. temperaturecooled
  4. filtrationIt is filtered
  5. customevaporated
  6. distillationthe residue distilled in a molecular still, and the fraction boiling at 155°-165°/0.1 mmHg
  7. customcollected as colorless oil