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
To a mixture of 150 g of N-(2-chloroethyl)-N'-(3-pyridyl) urea dissolved in 500 ml of tetrhydrofuran and 500 ml of dimethylformamide, 31.6 g of sodium hydride (60% oily suspension) was added under ice-cooling over 20 minutes. After stirring under ice-cooling for 10 minutes and at room temperature for 2 hours, 10 ml of acetic acid was added and the solvent was distilled off. Saturated saline water and chloroform were added to thr residue and insolubles were separated by filtration. The chloroform layer was washed with sodium hydrogen carbonate solution, dried and the solvent was distilled off. The residue was recrystallized from a mixture of chloroform and hexane to give 108.5 g of 1-(3-pyridyl)-2-imidazolidinone.
WORKUP
后处理
- additionwas added under ice-
- temperaturecooling over 20 minutes
- distillationthe solvent was distilled off
- additionSaturated saline water and chloroform were added to thr residue and insolubles
- customwere separated by filtration
- washThe chloroform layer was washed with sodium hydrogen carbonate solution
- customdried
- distillationthe solvent was distilled off
- customThe residue was recrystallized from a mixture of chloroform and hexane