Réaction #1552118

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 hemisulfate salt

Solvants

acetonitrile

Conditions de réaction

Traitement

1. 1
   AutrePrecipitation
2. 2
   FiltrationThe resulting yellow solid was recovered by filtration
3. 3
   workup.ADDITIONAcetone was added to the solid
4. 4
   workup.WAITThis mixture was slurried for 4 h
5. 5
   Filtrationthe solid was collected by centrifuge filtration (10,000 rpm for 1 min)
6. 6
   AutreThe white upper portion of the filter cake was removed
7. 7
   Autreair-dried overnight

Mode opératoire

(R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine hemisulfate salt was prepared by the drop-wise addition of 0.5 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 yellow solid was recovered by filtration. Acetone was added to the solid followed by sufficient water to cause dispersal (<5%). This mixture was slurried for 4 h and the solid was collected by centrifuge filtration (10,000 rpm for 1 min). The filtrate contained an oil droplet and the filter cake had a small amount of color at the bottom. The white upper portion of the filter cake was removed and air-dried overnight to leave the title salt as a white solid. (R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine hemisulfate salt had an extrapolated melting onset temperature by DSC of about 79° C.

Source