反应详情

温度

25 °C

To a suspension of 3-(3-(4-(pyridin-2-yloxymethyl)-benzyl)-isoxazol-5-yl)-pyridin-2-ylamine (500 mg) in methanol (2 mL) was added concentrated hydrochloric acid (123 μL) dropwise at 25° C, and the suspension turned into a solution. After adding tert-butyl methyl ether (2 mL) dropwise for 20 minutes at the same temperature and seeding, crystals precipitated. After stirring at 25° C for 10 minutes, tert-butyl methyl ether (6 mL) was added dropwise for 30 minutes, and the mixture was stirred at the same temperature for two hours. The precipitated crystals were filtered and dried to obtain the title compound (513 mg) as a white crystal.

1. customprecipitated
2. additiontert-butyl methyl ether (6 mL) was added dropwise for 30 minutes
3. stirringthe mixture was stirred at the same temperature for two hours
4. filtrationThe precipitated crystals were filtered
5. customdried