反应详情

A mixture of 4.0 g of 2-amino-N-[3-(1H-imidazol-1-yl)propyl]benzamide and 15 ml of ethyl chloroformate was heated in an oil bath at 95°-105° C. for 1.5 hours, dissolved in 50 ml of ethanol, and concentrated. The residue was mixed with 100 ml of ethanol and 3.2 g of potassium hydroxide, heated at reflux temperature for 3 hours and concentrated. The residue was dissolved in water and acidified with acetic acid to pH 6-7. The white precipitate was separated by filtration and recrystallized from ethanol. The desired product melted at 197°-200° C.

1. temperaturewas heated in an oil bath at 95°-105° C. for 1.5 hours
2. concentrationconcentrated
3. additionThe residue was mixed with 100 ml of ethanol and 3.2 g of potassium hydroxide
4. temperatureheated
5. temperatureat reflux temperature for 3 hours
6. concentrationconcentrated
7. dissolutionThe residue was dissolved in water
8. customThe white precipitate was separated by filtration
9. customrecrystallized from ethanol