反応 #1552113

反応方程式

(±)-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

溶媒

acetonitrile

ethyl acetate

反応条件

後処理

1. 1
   workup.ADDITIONat 60° C., was added dropwise, in the corresponding solvent, with vigorous stirring
2. 2
   その他precipitated the salt and it
3. 3
   温度to cool
4. 4
   ろ過The resulting solids were recovered by filtration
5. 5
   その他air-dried in a fume hood overnight
6. 6
   その他by DSC of about 74° C.

実験手順

(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.

出典