HRID36275
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 135 mg (0.191 mmole) of 5-n-butyl-4-[[2'-[N-(2-chlorobenzoyl)sulfamoyl]-5'-ethylbiphenyl-4-yl]methyl]-2-(2-chloro-5-nitrophenyl)-2,4-dihydro-3H-1,2,4-triazol-3-one (from Step C), 10 mg of platinum oxide, and 2 mL of ethyl acetate was stirred under an atmosphere of hydrogen (balloon) for 1 day and then then filtered through Celite. The crude product was chromatographed on a column of silica gel (gradient elution with 0.5-4% MeOH in CH2Cl2) to give 81 mg (63%) of the title compound; homogeneous by TLC in 9:1CH2Cl2 --MeOH; m/e 678 (M+1)+.
WORKUP
后处理
- filtrationfiltered through Celite
- customThe crude product was chromatographed on a column of silica gel (gradient elution with 0.5-4% MeOH in CH2Cl2)