反応 #64548

反応方程式

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

NaOH

→

title compound

収率 84.0%

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

収率 84.0%

反応条件

後処理

1. 1
   濃縮concentrated to dryness
2. 2
   workup.DISSOLUTIONThe residue was dissolved in 1 mL of methanol
3. 3
   workup.ADDITIONacidified to approximately pH 1.5 by addition of 1N HCl (methanolic)
4. 4
   濃縮again concentrated
5. 5
   workup.DISSOLUTIONThe residue was dissolved in CHCl3
6. 6
   乾燥dried over Na2SO4
7. 7
   ろ過filtered through Celite
8. 8
   その他Evaporation of the solvent

実験手順

A solution of 71 mg (0.102 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 Example 65, Step D) in 0.7 mL (0.7 mmole) of 1N NaOH (methanolic) was stirred at 60° C. overnight and then concentrated to dryness. The residue was dissolved in 1 mL of methanol, acidified to approximately pH 1.5 by addition of 1N HCl (methanolic), and again concentrated. The residue was dissolved in CHCl3, dried over Na2SO4, and filtered through Celite. Evaporation of the solvent yielded 58 mg (84%) of the title compound as a white solid; nearly homogeneous by TLC in 9:1 CH2Cl2 --MeOH; mass spectrum (FAB) m/e 679 (M+1)+.

出典