Réaction #1552128

Équation de réaction

α-oxo-glutaric acid

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

α-Oxo-glutaric acid

→

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

Solvants

acetonitrile

acetonitrile

Conditions de réaction

Traitement

1. 1
   workup.ADDITIONwas added dropwise with vigorous stirring
2. 2
   AutrePrecipitation
3. 3
   Températureto cool
4. 4
   FiltrationThe resulting solid was recovered by filtration
5. 5
   Autreair-dried in a fume hood overnight
6. 6
   Autreby DSC of about 91° C.
7. 7
   Autreby DSC of about 113° C.

Mode opératoire

(R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine oxoglutarate salt solvate was prepared by addition of a molar equivalent of α-oxo-glutaric acid to a solution of (R)-8-chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine in acetonitrile at 60° C. α-Oxo-glutaric acid in acetonitrile at 60° C. was added dropwise with vigorous stirring. Precipitation occurred immediately and the suspension was allowed to cool and stir overnight. The resulting solid was recovered by filtration and air-dried in a fume hood overnight. (R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine oxoglutarate salt solvate had an extrapolated desolvation onset temperature by DSC of about 91° C., and a second endotherm with an extrapolated onset temperature by DSC of about 113° C.

Source