反应详情

温度

0 °C

To a solution of 6-(5-methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyridin-3-ylamine (150 mg, 0.53 mmol) in THF (4 mL) was added triethylamine (65 mg, 90 μL, 0.64 mmol) and the resulting mixture cooled to 0° C. with ice. Then a solution of acetyl chloride (50 mg, 50 μL) in THF (1 mL) was added and the resulting mixture allowed to warm up to room temperature over 1 h. The mixture was then filtered and the filtrate evaporated before being diluted with methanol and potassium carbonate (10 mg) added. After one hour at room temperature the mixture was extracted with dichloromethane. The combined organic layers were then washed with water and then dried over sodium sulfate, filtered and evaporated to afford the title compound (145 mg, 84%) which was obtained as white crystals. MS: m/e=324.0 [M+H]+.

1. temperatureto warm up to room temperature over 1 h
2. filtrationThe mixture was then filtered
3. customthe filtrate evaporated
4. additionbefore being diluted with methanol and potassium carbonate (10 mg)
5. additionadded
6. extractionAfter one hour at room temperature the mixture was extracted with dichloromethane
7. washThe combined organic layers were then washed with water
8. dry with materialdried over sodium sulfate
9. filtrationfiltered
10. customevaporated