Réaction #1552114

Équation de réaction

L-glutamic acid

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

L-glutamic 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 L-glutamate salt

Solvants

EtOH H2O

isopropyl acetate

H2O

isopropyl acetate

Conditions de réaction

Traitement

1. 1
   Autrefollowed by evaporation of the solvent overnight
2. 2
   Autreto produce a solid
3. 3
   Autreisolated by filtration
4. 4
   AutreThe product crystallized without the need for evaporation of the solvent
5. 5
   Autreby DSC of about 187° C.

Mode opératoire

(R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine L-glutamate salt was prepared by addition of L-glutamic acid (0.5-1 eq.) in hot EtOH/H2O (˜2:1) to a solution of (R)-8-chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine in isopropyl acetate, followed by evaporation of the solvent overnight to produce a solid. The solid was slurried in isopropyl acetate and then isolated by filtration. Alternatively, (R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine L-glutamate salt was prepared by addition of a solution of L-glutamic acid (1 eq.) in hot H2O to a solution of (R)-8-chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine. The product crystallized without the need for evaporation of the solvent. (R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine L-glutamate salt had an extrapolated melting onset temperature by DSC of about 187° C.

Source