反应详情

Ethyl 2-bromo-3-[4-methoxy-3-[N-[[4-(trifluoromethyl)phenyl]methyl]carbamoyl]phenyl]propanoate (1.00 g, 2.05 mmol; Example 37) and 56 ml of ethanol were mixed and, after sodium thioethoxide (268 mg, 2.55 mmol) was added under stirring, the mixture was refluxed for 1.5 hours. The reaction mixture was concentrated, water was added, and the solution was extracted with ethyl acetate. The extract was washed with brine, then dried over anhydrous magnesium sulfate and concentrated. The residue was purified by silica gel chromatography (eluate n-hexane:ethyl acetate=2:1 v/v) to obtain 3.4 g (43%) of the title compound as colorless crystals.

1. temperaturethe mixture was refluxed for 1.5 hours
2. concentrationThe reaction mixture was concentrated
3. additionwater was added
4. extractionthe solution was extracted with ethyl acetate
5. washThe extract was washed with brine
6. dry with materialdried over anhydrous magnesium sulfate
7. concentrationconcentrated
8. customThe residue was purified by silica gel chromatography (eluate n-hexane:ethyl acetate=2:1 v/v)