반응 #64548

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

NaOH

→

title compound

수율 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

수율 84.0%

반응 조건

후처리

1. 1
   농축concentrated 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
   농축again concentrated
5. 5
   workup.DISSOLUTIONThe residue was dissolved in CHCl3
6. 6
   건조dried over Na2SO4
7. 7
   여과filtered through Celite
8. 8
   기타Evaporation of the solvent

실험 절차

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)+.

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