反应详情

22.1 g (0.1 mol) of 1-(4-nitrophenyl)[1,4]diazepane, 8.3 g (0.06 mol) of potassium carbonate and 120 ml of dimethylformamide were mixed together in a reactor. 8.3 ml (0.11 mol) of chloroacetyl chloride were added to this stirred suspension, while maintaining the temperature between 15 and 25° C. After stirring for about ten hours at room temperature, 400 g of slightly hydrochloric ice-cold water were added to the mixture: a yellow gum crystallized. After filtering off by suction, washing with water and drying under vacuum over phosphorus pentoxide, 22.4 g of yellow crystals were obtained (yield=75%).

1. temperaturewhile maintaining the temperature between 15 and 25° C
2. addition400 g of slightly hydrochloric ice-cold water were added to the mixture
3. customa yellow gum crystallized
4. filtrationAfter filtering off by suction
5. washwashing with water
6. dry with materialdrying under vacuum over phosphorus pentoxide