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
CONDITIONS
反应条件
- 温度
- 120 °C
PROCEDURE
实验过程
An amount of 54.25 g (0.529 mol) of 2,2-difluoro-1-chloroethane, 9.1 g (0.066 mol) of potassium carbonate and 50 g (0.264 mol) of potassium phthalimide are dissolved in 237 g of N,N-dimethylformamide. The reaction mixture is stirred in an autoclave under pressure at 120° C. for 12 h. After the end of the reaction, cooling is carried out to ambient temperature and the solvent is exhaustively removed under vacuum. The remaining residue is treated with 250 ml of water and the solid is filtered off. The filter residue is washed twice with water and the product is dried under vacuum. An amount of 55.5 g of 2-(2,2-difluoroethyl)-1H-isoindole-1,3(2H)-dione with a purity of 96.5% is obtained. This corresponds to a yield of 95.8% of theory.
WORKUP
后处理
- customAfter the end of the reaction
- temperaturecooling
- customis carried out to ambient temperature
- customthe solvent is exhaustively removed under vacuum
- additionThe remaining residue is treated with 250 ml of water
- filtrationthe solid is filtered off
- washThe filter residue is washed twice with water
- customthe product is dried under vacuum