반응 #64537

반응 방정식

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

→

desired product

수율 186.7%

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

수율 186.7%

용매

n-butylamine

반응 조건

후처리

1. 1
   기타After removal of excess n-butylamine
2. 2
   기타chromatographed over silica gel (gradient elution with 0.5-5.0% MeOH/CH2Cl2)

실험 절차

A solution of 100 mg (0.14 mmole) of 5-n-butyl-2-[5-(carbomethoxy)-2-chlorophenyl]-4-[[2'-[N-(2-chlorobenzoyl)sulfamoyl]biphenyl-4-yl]methyl]-2,4-dihydro-3H-1,2,4-triazol-3-one (from Step D), in 1 mL of n-butylamine was stirred at 65° C. overnight. After removal of excess n-butylamine, the crude product was flash chromatographed over silica gel (gradient elution with 0.5-5.0% MeOH/CH2Cl2) to give 96 mg (91%) of the desired product as a white solid, mp >155° C. (gradual), homogeneous by TLC in 95:5 CH2Cl2 --MeOH; mass spectrum (FAB) m/e 734 (M+1)+.

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