反应详情

To 4-[(E)-3-(3,5-Dichloro-phenyl)-4,4,4-trifluoro-but-2-enoyl]-2-methyl-benzoic acid tert-butyl ester (25 g) was added thioacetic acid (6 eq.) and triethylamine (200 μL) The solution was stirred at room temperature 2 drops of triethylamine were added. After stirring at room temperature for 24 hours, the mixture was poured in a mixture of water and ethyl acetate, extracted with ethyl acetate and washed with brine. The collected organic phases were dried over magnesium sulfate, filtered and the filtrate was evaporated under vacuo. The residue was purified by chromatography on silica gel (eluent: cyclohexane/dichloromethane) to give 4-[3-(3,5-Dichloro-phenyl)-4,4,4-trifluoro-3-mercapto-butyryl]-2-methyl-benzoic acid tert-butyl ester (3.78 g) 1H NMR (CDCl3, 400 MHz): δ=7.89 (d, J=8.8 Hz, 1 H), 7.72-7.79 (m, 2 H), 7.53-7.57 (m, 2 H), 7.35 (t, J=1.8 Hz, 1 H), 4.30 (d, J=18.3 Hz, 1 H), 3.97 (d, J=18.3 Hz, 1 H), 3.30 (s, 1 H), 2.59-2.65 (m, 3 H), 1.58-1.66 (m, 10 H), 1.56 ppm (s, 1 H).

1. additionwere added
2. extractionextracted with ethyl acetate
3. washwashed with brine
4. dry with materialThe collected organic phases were dried over magnesium sulfate
5. filtrationfiltered
6. customthe filtrate was evaporated under vacuo
7. customThe residue was purified by chromatography on silica gel (eluent: cyclohexane/dichloromethane)