反应详情

温度

150 °C

4-Amino-3-(2-cyclohexyl-1H-imidazol-1-yl)-N-(2-ethoxyethyl)-N-methylbenzamide as synthesized in Production Example 50, 2.51 g, 1,1′-carbonyldiimidazole 1.32 g and chlorobenzene 32 mL were mixed, and under nitrogen atmosphere, the temperature outside the reactor was heated to 150° C. for 16 hours. Allowing the reaction liquid to cool off, the solvent was distilled off therefrom. To the residue ethyl acetate and brine were added and the organic layer was separated. The organic layer was washed with saturated brine and dried over magnesium sulfate. After distilling the solvent off, the residue was crystallized from t-butyl methyl ether. Further heat-suspending the crystals in ethyl acetate for purification, 993 mg of the title compound was obtained.

1. additionwere mixed
2. customAllowing the reaction liquid
3. temperatureto cool off
4. distillationthe solvent was distilled off
5. additionTo the residue ethyl acetate and brine were added
6. customthe organic layer was separated
7. washThe organic layer was washed with saturated brine
8. dry with materialdried over magnesium sulfate
9. distillationAfter distilling the solvent off, the residue
10. customwas crystallized from t-butyl methyl ether
11. customfor purification