HRID2419646
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 9.1 grams (0.0294 mole) of α-(1-hydroxy-2-methyl-3-oxoisoindolin-1-yl)-N-methyl-o-toluamide and 180 milliliters of 2 M sulfuric acid is refluxed for 20 hours. The mixture is cooled and the solid separated by filtration. The solid is then dissolved in methylene chloride and washed twice with water and once with brine. The organic phase is dried over magnesium sulfate, filtered and evaporated in vacuo. The resulting oil is crystallized from ethanol to give 2,2'-dimethyl spiro[isoindolin-1,3'(4'H)-isoquinoline]1',3-dione, m.p. 202° - 203° C.
WORKUP
后处理
- temperatureis refluxed for 20 hours
- temperatureThe mixture is cooled
- customthe solid separated by filtration
- dissolutionThe solid is then dissolved in methylene chloride
- washwashed twice with water and once with brine
- dry with materialThe organic phase is dried over magnesium sulfate
- filtrationfiltered
- customevaporated in vacuo
- customThe resulting oil is crystallized from ethanol