反应详情

3-Amino-5-chloro-2-(2-cyclohexyl-1H-imidazol-1-yl)pyridine as synthesized in Production Example 103, 838 mg, 1,1′-carbonyldi-imidazole 983 mg and 1,2-chlorobenzene 25 mL were mixed and heated under reflux for 15 hours. Cooling the reaction liquid off, the precipitate was recovered by filtration and washed with methanol. The resulting crystals were dissolved in a liquid mixture of 2N hydrochloric acid and methanol, and the insoluble matter was separated by filtration. The filtrate was made weakly alkaline with saturated aqueous sodium hydrogencarbonate solution, and the precipitate was recovered by filtration. Drying the same in flowing air under heating, 620 mg of the title compound was obtained.

1. additionwere mixed
2. temperatureheated
3. temperatureunder reflux for 15 hours
4. temperatureCooling
5. customthe reaction liquid off, the precipitate
6. filtrationwas recovered by filtration
7. washwashed with methanol
8. dissolutionThe resulting crystals were dissolved in a liquid mixture of 2N hydrochloric acid and methanol
9. customthe insoluble matter was separated by filtration
10. filtrationthe precipitate was recovered by filtration
11. customDrying the same
12. temperatureunder heating