Réaction #1552125

ord-551bd28d46fd4e4d8e7b1635ee8dcd82

Équation de réaction

O=C(O)CC(O)(CC(=O)O)C(=O)O
citric acid
C[C@H]1CNCCc2ccc(Cl)cc21
(R)-8-chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine
CO
MeOH
→
C[C@H]1CNCCc2ccc(Cl)cc21.C[C@H]1CNCCc2ccc(Cl)cc21.O.O=C(O)CC(O)(CC(=O)O)C(=O)O.O=C(O)CC(O)(CC(=O)O)C(=O)O
(R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine citrate salt hemihydrate

Réactifs

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

Réactifs

Aucun

Solvants

CC(=O)OC(C)C
isopropyl acetate

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    AutrePrecipitation
  2. 2
    Autreby DSC of about 80° C.

Mode opératoire

(R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine citrate salt hemihydrate was prepared by dropwise addition of 1 mole equivalent of citric acid in hot MeOH to a solution of (R)-8-chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine in isopropyl acetate. Precipitation occurred spontaneously. (R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine citrate salt hemihydrate had a dehydration onset temperature by DSC of about 80° C.

Source

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