反应详情

温度

60 °C

To a solution of 4-mercapto-phenyl acetic acid (30 g, 178.34 mmol) in methanol (60 ml) was added sulfuric acid (9.5 mL, 178.34 mmol) dropwise. Reaction mixture was then heated at 60° C. for 3 hr, concentrated to remove methanol. The residue was neutralized with satd. aq. NaHCO3 solution and extracted with ethyl acetate (3×30 mL) washed with brine, dried over anhydrous sodium sulfate, filtered and concentrated. Product was purified using column chromatography in 1% ethyl acetatae:hexane as eluent which afforded (4-mercapto-phenyl)-acetic acid methyl ester (27 g).

1. customReaction mixture
2. concentrationconcentrated
3. customto remove methanol
4. extractionaq. NaHCO3 solution and extracted with ethyl acetate (3×30 mL)
5. washwashed with brine
6. dry with materialdried over anhydrous sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated
9. customProduct was purified