반응 #1782678

반응 방정식

5-{[3-(4-Fluoro-phenyl)-5-methyl-isoxazol-4-ylmethyl]-amino}-2H-pyrazole-3-carboxylic acid methyl ester

lithium hydroxide monohydrate

→

5-{[3-(4-fluoro-phenyl)-5-methyl-isoxazol-4-ylmethyl]-amino}-2H-pyrazole-3-carboxylic acid

수율 91.0%

용매

THF

water

반응 조건

후처리

1. 1
   기타After evaporation the mixture
2. 2
   workup.ADDITIONwas diluted with water (10 mL) and citric acid (10%)
3. 3
   추출extracted with ethyl acetate (2×80 mL)
4. 4
   건조The combined extracts were then dried with sodium sulfate
5. 5
   여과filtered
6. 6
   기타evaporated

실험 절차

5-{[3-(4-Fluoro-phenyl)-5-methyl-isoxazol-4-ylmethyl]-amino}-2H-pyrazole-3-carboxylic acid methyl ester (900 mg, 2.72 mmol) was then dissolved in THF (20 mL) and lithium hydroxide monohydrate (686 mg, 16.34 mmol) in water (15 mL) added and the resulting mixture stirred for 12 h. After evaporation the mixture was diluted with water (10 mL) and citric acid (10%) and extracted with ethyl acetate (2×80 mL). The combined extracts were then dried with sodium sulfate, filtered and evaporated to afford 5-{[3-(4-fluoro-phenyl)-5-methyl-isoxazol-4-ylmethyl]-amino}-2H-pyrazole-3-carboxylic acid (703 mg, 91%) as an off white solid. MS: m/e=317.4 [M+H]+.

출처