HRID1197775

反应详情

EQUATION

反应方程式

HRID 1197775 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 211 mg 8-acetyl-7,8-dihydro-6,6-dimethyl-6H-[1,2,5]oxadiazolo[3,4-g][1,4]benzoxazine 3-oxide, 15 ml toluene and 0.18 ml triethyl phosphite was heated under reflux for 16 hours, the solvent was distilled off from the reaction mixture, diethyl ether was added to the residue, and the precipitate was collected by filtration and recrystallized from 2 ml ethanol, giving 136 mg of 8-acetyl-7,8-dihydro-6,6-dimethyl-6H-[1,2,5]oxadiazolo[3,4-g][1,4]benzoxazine.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 16 hours
  3. distillationthe solvent was distilled off from the reaction mixture, diethyl ether
  4. additionwas added to the residue
  5. filtrationthe precipitate was collected by filtration
  6. customrecrystallized from 2 ml ethanol