Réaction #1552117

Équation de réaction

sulfuric acid

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

isopropyl acetate

→

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

Solvants

acetonitrile

Conditions de réaction

Traitement

1. 1
   AutrePrecipitation
2. 2
   FiltrationThe resulting solid was recovered by filtration
3. 3
   Autreby DSC of about 162° C.

Mode opératoire

(R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine bisulfate salt was prepared by drop-wise addition of 1 mole equivalent of concentrated sulfuric acid to a solution of (R)-8-chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine free base in either isopropyl acetate or acetonitrile with vigorous stirring. Precipitation occurred immediately and the suspension was allowed to stir for 1 to 2 days. The resulting solid was recovered by filtration. (R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine bisulfate salt had an extrapolated melting onset temperature by DSC of about 162° C.

Source