Réaction #1552113

Équation de réaction

(±)-mandelic acid

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

acetone

(±)-Mandelic acid

water

→

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

Solvants

acetonitrile

ethyl acetate

Conditions de réaction

Traitement

1. 1
   workup.ADDITIONat 60° C., was added dropwise, in the corresponding solvent, with vigorous stirring
2. 2
   Autreprecipitated the salt and it
3. 3
   Températureto cool
4. 4
   FiltrationThe resulting solids were recovered by filtration
5. 5
   Autreair-dried in a fume hood overnight
6. 6
   Autreby DSC of about 74° C.

Mode opératoire

(R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine (±)-mandelate salt hydrate was prepared by the addition of one equivalent of (±)-mandelic acid to a solution of (R)-8-chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine in acetonitrile, ethyl acetate, or acetone at 60° C. (±)-Mandelic acid, at 60° C., was added dropwise, in the corresponding solvent, with vigorous stirring. Addition of water to these three samples precipitated the salt and it was allowed to cool and stir overnight. The resulting solids were recovered by filtration and air-dried in a fume hood overnight. (R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine (±)-mandelate salt hydrate had an extrapolated desolvation onset temperature by DSC of about 74° C.

Source