Réaction #1552121

ord-8fe9edbace3c42fe91f9e72c24b9408e

Équation de réaction

O=C(O)CCCCC(=O)O
adipic acid
C[C@H]1CNCCc2ccc(Cl)cc21
(R)-8-chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine
→
C[C@H]1CNCCc2ccc(Cl)cc21.O=C(O)CCCCC(=O)O
(R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine adipate salt

Réactifs

O=C(O)CCCCC(=O)O
adipic acid
C[C@H]1CNCCc2ccc(Cl)cc21
(R)-8-chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine

Réactifs

Aucun

Solvants

CC(C)=O
acetone

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    AutrePrecipitation
  2. 2
    Autrestarting at onset temperatures between 104° C. and 107° C.

Mode opératoire

(R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine adipate salt was prepared by addition of adipic acid (0.5-1 eq.) in acetone to a solution of (R)-8-chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine at ˜62° C. Precipitation occurred within 5 min and the suspension was allowed to cool to ambient temperature with stirring. (R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine adipate salt had multiple endothermic events by DSC starting at onset temperatures between 104° C. and 107° C.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08999970B2uspto-grants-2015_04