反应详情

温度

0 °C

A solution of benzoyl chloride (0.36 g) in dichloromethane (1.5 ml) was added dropwise to a mixture of 2-[3-(imidazol-1-yl)propylamino]-2-methyl-1-propanol (0.5 g) and triethylamine (0.5 g) in dichloromethane (5 ml) with stirring under nitrogen at 0° C. The mixture was stirred at 0° C. for 1 hour and then allowed to warm up to ambient temperature and stirred at this temperature for 3 hours. Saturated aqueous sodium bicarbonate (5 ml) was added. The mixture was shaken and the organic layer separated. The aqueous layer was extracted with further dichloromethane. The combined organic extracts were dried, filtered and evaporated to give an oil which was dissolved in ether and treated with ethereal hydrogen chloride to give 2-[3-(imidazol-1-yl)propylamino]-2,2-dimethylethyl benzoate dihydrochloride, m.p. 198-199° C., after recrystallisation from ethanol.

1. stirringThe mixture was stirred at 0° C. for 1 hour
2. temperatureto warm up to ambient temperature
3. stirringstirred at this temperature for 3 hours
4. stirringThe mixture was shaken
5. customthe organic layer separated
6. extractionThe aqueous layer was extracted with further dichloromethane
7. customThe combined organic extracts were dried
8. filtrationfiltered
9. customevaporated
10. customto give an oil which