Réaction #1552120

Équation de réaction

HBr

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

isopropyl acetate

→

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

Solvants

ethyl acetate

acetonitrile

ethyl acetate

Conditions de réaction

Traitement

1. 1
   AutreThe product readily precipitated from the reaction in isopropyl acetate
2. 2
   AutreIn acetonitrile the solvent was evaporated
3. 3
   Autreto obtain a solid
4. 4
   Autrecrystallization
5. 5
   AutreThe reaction was then closed
6. 6
   workup.STIRRINGstirring
7. 7
   Autreto afford a yellow suspension
8. 8
   FiltrationThe suspension was filtered
9. 9
   Lavagethe solid was washed with cold ethyl acetate
10. 10
    Autrewas under nitrogen at ˜38° C.
11. 11
    Autreby TGA of about 72.5° C.

Mode opératoire

(R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine hydrobromide salt hemihydrate was prepared by the dropwise addition of one equivalent of aqueous HBr (˜48%) to a solution of (R)-8-chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine free base in isopropyl acetate, acetonitrile, or ethyl acetate with vigorous stirring. The product readily precipitated from the reaction in isopropyl acetate. In acetonitrile the solvent was evaporated to near dryness to obtain a solid. In ethyl acetate, seeds were added and the reaction was allowed to stir unstoppered to initiate crystallization. The reaction was then closed and stirring was continued to afford a yellow suspension. The suspension was filtered and the solid was washed with cold ethyl acetate. The resulting white solid was under nitrogen at ˜38° C., and held overnight at 25° C./75% RH. (R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine hydrobromide salt hemihydrate had an extrapolated dehydration onset temperature by TGA of about 72.5° C.

Source