HRID250365
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 160 ml of butanol, 20.0 g of (1,3-dioxo-1,3-dihydro-isoindol-2-yl)-acetic acid (94.6 mmol) and 2.0 ml of concentrated sulfuric acid was refluxed with stirring for 24 h. Then 5 g of sodium bicarbonate were added in portions, stirring continued at r.t. for 5 min and the solvent evaporated in vacuo. The residue was partitioned between 100 ml of water and 100 ml of ethyl acetate. The organic phase was washed with 100 ml of brine, dried over sodium sulfate and was evaporated in vacuo to give a yellowish oil that later solidified. 24.02 g of the title compound were obtained; MS-(+)-ion: M+1=261.9.
WORKUP
后处理
- temperaturewas refluxed
- stirringstirring
- waitcontinued at r.t. for 5 min
- customthe solvent evaporated in vacuo
- customThe residue was partitioned between 100 ml of water and 100 ml of ethyl acetate
- washThe organic phase was washed with 100 ml of brine
- dry with materialdried over sodium sulfate
- customwas evaporated in vacuo
- customto give a yellowish oil that