反応 #1552112

反応方程式

trans-cinnamic 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 trans-cinnamate salt

溶媒

acetonitrile

反応条件

後処理

1. 1
   その他at 50° C
2. 2
   温度The sample was cooled slowly
3. 3
   その他The resulting white solid was isolated by filtration
4. 4
   その他dried
5. 5
   その他Similar samples prepared in isopropanol
6. 6
   その他acetone or THF produced white solids only after removal of solvent and trituration with MTBE
7. 7
   その他by DSC of 106° C.

実験手順

(R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine trans-cinnamate salt was prepared by combining one equivalent of trans-cinnamic acid with (R)-8-chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine in acetonitrile at 50° C. The sample was cooled slowly and stirred overnight. The resulting white solid was isolated by filtration and dried. Similar samples prepared in isopropanol, acetone or THF produced white solids only after removal of solvent and trituration with MTBE. (R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine trans-cinnamate salt had an extrapolated melting onset temperature by DSC of 106° C.

出典