反応 #1552109

反応方程式

(R)-8-chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine

fumaric acid

water

EtOH

→

(R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine hemifumarate salt

溶媒

isopropyl acetate

反応条件

後処理

1. 1
   その他A suspension resulted
2. 2
   その他the heat source was removed
3. 3
   温度to cool to ambient temperature
4. 4
   ろ過The suspension was filtered
5. 5
   洗浄the solid was washed with isopropyl acetate
6. 6
   その他dried on the filter
7. 7
   その他by DSC of 158° C.

実験手順

(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.

出典