HRID1197775
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas heated
- temperatureunder reflux for 16 hours
- distillationthe solvent was distilled off from the reaction mixture, diethyl ether
- additionwas added to the residue
- filtrationthe precipitate was collected by filtration
- customrecrystallized from 2 ml ethanol