반응 #1971455

반응 방정식

3-{4-[4-(4-tert-Butylphenyl)-4-oxo-2-(4-trifluoromethoxyphenyl)butyryl]benzoylamino}propionic acid methyl ester

NaOH

→

title compound

수율 39.3%

3-{4-[4-(4-tert-Butylphenyl)-4-oxo-2-(4-trifluoromethoxyphenyl)butyryl]benzoylamino}propionic acid

수율 39.3%

용매

ethanol

반응 조건

후처리

1. 1
   농축The reaction mixture was concentrated in vacuo
2. 2
   workup.ADDITIONadded hydrochloric acid (4N, 34 mL) to pH 1-2
3. 3
   여과After 1 h the precipitate was filtered
4. 4
   세척washed carefully with water
5. 5
   기타dried
6. 6
   기타The residue was purified by preparative HPLC

실험 절차

3-{4-[4-(4-tert-Butylphenyl)-4-oxo-2-(4-trifluoromethoxyphenyl)butyryl]benzoylamino}propionic acid methyl ester (12 g, 21 mmol) was dissolved in ethanol 96% (250 mL), added 4N NaOH (31.2 mL, 125 mmol), and stirred for 2 h 45 min. The reaction mixture was concentrated in vacuo and the residue suspended in water (150 mL) and added hydrochloric acid (4N, 34 mL) to pH 1-2. After 1 h the precipitate was filtered and washed carefully with water and dried. The residue was purified by preparative HPLC using acetonitrile (gradient from 42% to 97.5%), water and TFA (2.5%) as eluent to afford 4.7 g of the title compound.

출처