反応 #64531

反応方程式

2-(5-amino-2-chlorophenyl)-5-n-butyl-4-[[2'-[N-(2-chlorobenzoyl)sulfamoyl]biphenyl-4-yl]methyl]-2,4-dihydro-3H-1,2,4-triazol-3-one

sodium hydride

valeryl chloride

→

desired compound

5-n-Butyl-4-[[2'-[N-(2-chlorobenzoyl)sulfamoyl]biphenyl-4-yl]methyl]-2-[2-chloro-5-(valerylamino)phenyl]-2,4-dihydro-3H-1,2,4-triazol-3-one

反応条件

後処理

1. 1
   その他chromatographed over silica gel (gradient elution with 0.5-2.0% MeOH/CH2Cl2)

実験手順

The title compound was prepared from 2-(5-amino-2-chlorophenyl)-5-n-butyl-4-[[2'-[N-(2-chlorobenzoyl)sulfamoyl]biphenyl-4-yl]methyl]-2,4-dihydro-3H-1,2,4-triazol-3-one (from Example 60), sodium hydride, and valeryl chloride according the procedure of Example 57. The crude product was flash chromatographed over silica gel (gradient elution with 0.5-2.0% MeOH/CH2Cl2) to give the desired compound as a cream-colored solid in 48% yield, mp >110° C. (gradual), homogeneous by TLC (9:1 MeOH/CH2Cl2), mass spectrum (FAB) m/e 734 (M+1)+.

出典