反应详情

To a solution of (3-(3-pyridyloxy)propyl)methylamine (800.0 mg, 4.81 mmol) in ethanol (12 mL) was added galactaric acid (505.7 mg, 2.41 mmol). Water (2.5 mL) was added dropwise, while gently warming the light-yellow solution. To remove some white, insoluble solids, the warm solution was filtered through a glass wool plug, washing the filter plug with a warm solution of ethanol-water (4:1, v/v) (4 mL). The filtrate was diluted with ethanol (18 mL), producing a white precipitate. The mixture was allowed to cool to ambient temperature and was further cooled at 5° C. for 15 h. The precipitate was filtered, washed with ethanol (6 mL), vacuum dried at 45° C. for 10 h, followed by further vacuum drying at ambient temperature for 48 h to give 994.4 mg (76.1%) of an off-white, crystalline powder, mp 161-165.5° C.

1. temperaturewhile gently warming the light-yellow solution
2. customTo remove some white, insoluble solids
3. filtrationthe warm solution was filtered through a glass wool plug
4. washwashing the filter plug with a warm solution of ethanol-water (4:1
5. additionThe filtrate was diluted with ethanol (18 mL)
6. customproducing a white precipitate
7. temperaturewas further cooled at 5° C. for 15 h
8. filtrationThe precipitate was filtered
9. washwashed with ethanol (6 mL), vacuum
10. customdried at 45° C. for 10 h
11. customdrying at ambient temperature for 48 h
12. customto give 994.4 mg (76.1%) of an off-white, crystalline powder, mp 161-165.5° C.