反应详情

8.95 g of 4-[4-((R)-3-chloro-2-hydroxy-propylamino)-phenyl]-morpholin-3-one (MW=284.75; 1 eq.) were added to 189 g of conc. aqueous ammonia (MW=17.03; 88 eq.). The reaction mixture was stirred for 4 h at room temperature. Then 0.9 g of charcoal were added and after 10 min of stirring, the suspension was filtered and the cake washed with 30 mL of water. Filtrate and wash water were combined and concentrated in vacuo. To the residue were added 50 mL of ethanol. The resulting suspension was stirred for 1 h at ambient temperature and then cooled to 0° C. After stirring for at least 2 h at this temperature, the product was isolated by filtration and the filter cake was washed with 25 mL of ethanol. After drying in vacuo at 30° C., 5.73 g of the crystalline title compound were isolated. Yield=60.4%.

1. stirringof stirring
2. filtrationthe suspension was filtered
3. washthe cake washed with 30 mL of water
4. washFiltrate and wash water
5. concentrationconcentrated in vacuo
6. additionTo the residue were added 50 mL of ethanol
7. stirringThe resulting suspension was stirred for 1 h at ambient temperature
8. temperaturecooled to 0° C
9. stirringAfter stirring for at least 2 h at this temperature
10. customthe product was isolated by filtration
11. washthe filter cake was washed with 25 mL of ethanol
12. customAfter drying in vacuo at 30° C.