反应详情

温度

130 °C

A mixture of 1.40 g of methyl 5-(3H-imidazo[4,5-c]pyridin-3-yl)-3-{[2-(trifluoromethyl)benzyl]oxy}thiophene-2-carboxylate (compound B1b) and 65 ml of a saturated solution of ammonia in methanol were stirred in an autoclave at 130° C. for 7 h. The mixture was allowed to cool down to room temperature and concentrated to about half of the volume. The precipitated solid was filtered, widely dissolved in 500 ml of methanol upon heating and filtered again. The filtrate was concentrated to about 25 ml upon which solid precipitated. It was filtered, dissolved in acetonitrile containing small amounts of water and finally the solution was lyophilized to give the title compound as a colorless powder.

1. temperatureto cool down to room temperature
2. concentrationconcentrated to about half of the volume
3. filtrationThe precipitated solid was filtered
4. dissolutionwidely dissolved in 500 ml of methanol
5. temperatureupon heating
6. filtrationfiltered again
7. concentrationThe filtrate was concentrated to about 25 ml upon which solid
8. customprecipitated
9. filtrationIt was filtered
10. dissolutiondissolved in acetonitrile containing small amounts of water