Réaction #1552109

Équation de réaction

(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

Solvants

isopropyl acetate

Conditions de réaction

Traitement

1. 1
   AutreA suspension resulted
2. 2
   Autrethe heat source was removed
3. 3
   Températureto cool to ambient temperature
4. 4
   FiltrationThe suspension was filtered
5. 5
   Lavagethe solid was washed with isopropyl acetate
6. 6
   Autredried on the filter
7. 7
   Autreby DSC of 158° C.

Mode opératoire

(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.

Source