反応 #47122

反応方程式

potassium iodide

4-bromomethyl-2′-cyanobiphenyl

L-valine methyl ester

potassium carbonate

→

N-[(2′-cyanobiphenyl-4-yl)methyl]-(L)-valine methyl ester oxalate salt

溶媒

acetonitrile

反応条件

後処理

1. 1
   その他the solvent was removed under vacuum
2. 2
   workup.ADDITIONWater and xylene was added to reaction mass
3. 3
   その他the organic layer was separated
4. 4
   workup.ADDITIONA solution of oxalic acid was added to the organic layer
5. 5
   workup.STIRRINGstirred for about an hour at ambient temperature

実験手順

In one of the preferred embodiments 4-bromomethyl-2′-cyanobiphenyl, L-valine methyl ester, potassium carbonate and potassium iodide are taken in acetonitrile. The reaction mixture was stirred at about 40-45° C. for about 3 to 4 hours and the solvent was removed under vacuum. Water and xylene was added to reaction mass and the organic layer was separated. A solution of oxalic acid was added to the organic layer and stirred for about an hour at ambient temperature to give N-[(2′-cyanobiphenyl-4-yl)methyl]-(L)-valine methyl ester oxalate salt.

出典