반응 #41197

반응 방정식

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

LiOH

→

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

수율 89.0%

용매

methanol

water

반응 조건

후처리

1. 1
   온도at reflux overnight
2. 2
   농축the solution was concentrated under reduced pressure
3. 3
   기타to remove the methanol
4. 4
   workup.ADDITIONThe residue was diluted with water
5. 5
   추출The resulting mixture was then extracted with ethyl acetate three times
6. 6
   농축The combined organic extracts were concentrated in vacuo

실험 절차

To a solution of 1-cyclobutyl-5-trifluoromethyl-1H-pyrazole-4-carboxylic acid ethyl ester (117 mg, 0.45 mmol) in methanol (5 mL) and water (5 mL) was added LiOH (13 mg, 0.54 mmol). The reaction mixture was stirred at reflux overnight, and then the solution was concentrated under reduced pressure to remove the methanol. The residue was diluted with water and the solution was acidified to pH=2 with concentrated HCl. The resulting mixture was then extracted with ethyl acetate three times. The combined organic extracts were concentrated in vacuo to give 1-cyclobutyl-5-trifluoromethyl-1H-pyrazole-4-carboxylic acid (93 mg, 89%), which was used without further purification.

출처