反応 #1552110

反応方程式

Orotic acid

orotic acid

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

acetone

→

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

溶媒

isopropanol

ethyl acetate

反応条件

後処理

1. 1
   その他Precipitation
2. 2
   温度to cool
3. 3
   ろ過The resulting solid was recovered by filtration
4. 4
   その他air-dried in a fume hood overnight
5. 5
   その他by DSC of 236° C.

実験手順

(R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine orotate salt was prepared by addition of one equivalent of orotic acid to a solution of (R)-8-chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine in isopropanol, ethyl acetate, or acetone at 60° C. Orotic acid, at 60° C., was added drop-wise, in the corresponding solvent, with vigorous stirring. Precipitation occurred immediately and the suspension was allowed to cool and stir overnight. The resulting solid was recovered by filtration and air-dried in a fume hood overnight. (R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine orotate salt had an extrapolated initial melting onset temperature by DSC of 236° C.

出典