反应详情

温度

40 °C

To 3-(3-(4-(pyridin-2-yloxymethyl)-benzyl)-isoxazol-5-yl)-pyridin-2-ylamine (1 g) was added methanol (4 mL). While heating and stirring at 40° C, to this suspension was added a solution of concentrated sulfuric acid (79.4 μL) in methanol (1 mL) dropwise, which turned into a solution. After stirring at 40° C for 10 minutes and seeding, crystals precipitated. After stirring at 40° C for 20 minutes, tert-butyl methyl ether (25 mL) was added dropwise at the same temperature for one hour, followed by slow cooling, then stirring at 23° C for three hours. The precipitated crystals were filtered and dried to obtain the title compound (1.04 g).

1. temperatureWhile heating
2. stirringAfter stirring at 40° C for 10 minutes
3. customseeding, crystals precipitated
4. stirringAfter stirring at 40° C for 20 minutes
5. additiontert-butyl methyl ether (25 mL) was added dropwise at the same temperature for one hour
6. stirringstirring at 23° C for three hours
7. filtrationThe precipitated crystals were filtered
8. customdried