反应详情

Ethyl 3-[1-(2-amino-4-methylphenyl)-1H-imidazol-2-yl]-propanoate as synthesized in above Example 181, 160 mg, 1,1′-carbonyldiimidazole 143 mg and 1,2-dichlorobenzene 6 mL were mixed and heated under reflux for 1.5 hours. The reaction liquid was allowed to cool off, and the precipitate was recovered by filtration and washed with ethyl acetate. After being dried under reduced pressure, the product was mixed with 3 mL of ethanol and 3.0 mL of 1N aqueous sodium hydroxide solution and heated under reflux for 20 minutes. Cooling the reaction liquid off, 3.0 mL of 1N hydrochloric acid was added. The precipitated crystals were recovered by filtration, washed with water and dried in flowing air under heating to provide 82 mg of the title compound.

1. additionwere mixed
2. temperatureheated
3. temperatureunder reflux for 1.5 hours
4. customThe reaction liquid
5. temperatureto cool off
6. filtrationthe precipitate was recovered by filtration
7. washwashed with ethyl acetate
8. customAfter being dried under reduced pressure
9. additionthe product was mixed with 3 mL of ethanol and 3.0 mL of 1N aqueous sodium hydroxide solution
10. temperatureheated
11. temperatureunder reflux for 20 minutes
12. temperatureCooling
13. customthe reaction liquid off, 3.0 mL of 1N hydrochloric acid
14. additionwas added
15. filtrationThe precipitated crystals were recovered by filtration
16. washwashed with water
17. customdried
18. temperatureunder heating