反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A mixture of 5.53 g 2-(4-hydroxypyrrolidin-2-on-1-yl) acetamide and 44.3 ml acetyl chloride is refluxed for 15 minutes. It is then cooled, the solvent is evaporated in vacuo and the residue oil taken up with a small quantity of aqueous sodium bicarbonate, and solid sodium bicarbonate is added under stirring until neutrality. Most of the water contained in the mixture is removed by treatment in vacuo with methylisobutylketone, the residue is taken up with methylene chloride, made anhydrous over sodium sulphate and evaporated in vacuo. The residue oil is slurried into isopropyl alcohol/ethyl ether and crystallized from isopropyl alcohol/isopropyl ether (20:80) to obtain 2-(4-acetoxypyrrolidin-2-on-1-yl) acetamide, which purified by chromatography melts at 84°-86° C.
WORKUP
后处理
- temperatureis refluxed for 15 minutes
- temperatureIt is then cooled
- customthe solvent is evaporated in vacuo
- additionis added
- customis removed by treatment in vacuo with methylisobutylketone
- customevaporated in vacuo
- customcrystallized from isopropyl alcohol/isopropyl ether (20:80)