反应详情

温度

60 °C

(R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine hemifumarate salt was prepared by dropwise addition of a half-molar amount of fumaric acid in 1:1 water:EtOH (˜0.6 M) to a solution of (R)-8-chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine in isopropyl acetate with vigorous stirring. A suspension resulted. It was heated to 60° C., held at that temperature for 1 h, and then the heat source was removed and the sample was allowed to cool to ambient temperature while stirring overnight. The suspension was filtered and the solid was washed with isopropyl acetate and dried on the filter. (R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine hemifumarate salt had an extrapolated melting onset temperature by DSC of 158° C.

1. customA suspension resulted
2. customthe heat source was removed
3. temperatureto cool to ambient temperature
4. filtrationThe suspension was filtered
5. washthe solid was washed with isopropyl acetate
6. customdried on the filter
7. customby DSC of 158° C.