Réaction #1552112

Équation de réaction

trans-cinnamic acid

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

→

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

Solvants

acetonitrile

Conditions de réaction

Traitement

1. 1
   Autreat 50° C
2. 2
   TempératureThe sample was cooled slowly
3. 3
   AutreThe resulting white solid was isolated by filtration
4. 4
   Autredried
5. 5
   AutreSimilar samples prepared in isopropanol
6. 6
   Autreacetone or THF produced white solids only after removal of solvent and trituration with MTBE
7. 7
   Autreby DSC of 106° C.

Mode opératoire

(R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine trans-cinnamate salt was prepared by combining one equivalent of trans-cinnamic acid with (R)-8-chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine in acetonitrile at 50° C. The sample was cooled slowly and stirred overnight. The resulting white solid was isolated by filtration and dried. Similar samples prepared in isopropanol, acetone or THF produced white solids only after removal of solvent and trituration with MTBE. (R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine trans-cinnamate salt had an extrapolated melting onset temperature by DSC of 106° C.

Source