반응 #48588

반응 방정식

4-(2,6-difluoro-benzoylamino)-1H-pyrazole-3-carboxylic acid ethyl ester

→

4-(2,6-difluoro-benzoylamino)-1H-pyrazole-3-carboxylic acid

수율 61.7%

용매

NaOH MeOH

반응 조건

후처리

1. 1
   기타Volatile materials were removed in vacuo, water (300 ml)
2. 2
   workup.ADDITIONadded
3. 3
   여과The resultant precipitate was collected by filtration
4. 4
   건조dried through azeotrope with toluene

실험 절차

A mixture of 4-(2,6-difluoro-benzoylamino)-1H-pyrazole-3-carboxylic acid ethyl ester (10.2 g) in 2 M aqueous NaOH/MeOH (1:1, 250 ml) was stirred at ambient temperature for 14 h. Volatile materials were removed in vacuo, water (300 ml) added and the mixture taken to pH 5 using 1M aqueous HCl. The resultant precipitate was collected by filtration and dried through azeotrope with toluene to afford 4-(2,6-difluoro-benzoylamino)-1H-pyrazole-3-carboxylic acid as a pink solid (5.70 g). (LC/MS: Rt 2.33, [M+H]+ 267.96).

출처