반응 #41199

반응 방정식

5-chloro-1-cyclobutyl-1H-pyrazole-4-carboxylic acid ethyl ester

LiOH

→

5-chloro-1-cyclobutyl-1H-pyrazole-4-carboxylic acid

수율 94.0%

용매

methanol

water

반응 조건

후처리

1. 1
   온도at reflux for 4 hours
2. 2
   농축concentrated under reduced pressure
3. 3
   기타to remove the methanol
4. 4
   workup.ADDITIONThe residue was diluted with water
5. 5
   추출extracted with ethyl acetate
6. 6
   기타The organic layer was evaporated in vacuo

실험 절차

To a solution of 5-chloro-1-cyclobutyl-1H-pyrazole-4-carboxylic acid ethyl ester (182 mg, 0.79 mmol) in methanol (8 mL) and water (8 mL) was added LiOH (23 mg, 0.96 mmol). The reaction mixture was stirred at reflux for 4 hours and then concentrated under reduced pressure to remove the methanol. The residue was diluted with water, acidified to pH 2 with concentrated HCl and extracted with ethyl acetate. The organic layer was evaporated in vacuo to give 5-chloro-1-cyclobutyl-1H-pyrazole-4-carboxylic acid (148 mg, 94%) which was used without further purification.

출처