Sodium hydride → 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

참여 물질

역할	이름	HCID	투입량
반응물	Sodium hydride	HCID 24758	—
반응물	Valeryl chloride	HCID 61186	—
반응물	4''-[1-(5-Amino-2-chloro-phenyl)-3-butyl-5-oxo-1,5-dihydro-[1,2,4]triazol-4-ylmethyl]-biphenyl-2-sulfonic acid 2-chloro-benzoylamide	HCID 10032193	—
생성물	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	HCID 10078663	—

반응 단계

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)+.

출처 및 근거

DOI	10.6084/m9.figshare.5104873.v1
특허 번호	US05411980
출처 데이터셋	uspto-grants-1995_05
ORD ID	ord-e3472501156347b7b2f8f4a608c55708
출처 메모	uspto-grants-1995_05