反应详情

温度

95 °C

To a solution 2-methyl-4-trifluoromethylsulfoxyindole (3.2 g; prepared in Reference Example 2) in N,N-dimethylformamide (50 ml) was added acrylic acid methyl ester (2.24 ml), diisopropylethylamine (5.9 ml) and dichlorobis(triphenylphosphine)palladium(II) (238 mg), and the mixture was stirred at 95° C. for 2 days. To the reaction mixture was added water and ethyl acetate, then separated. The aqueous layer was extracted with ethyl acetate. The combined organic layer was washed with water and a saturated aqueous solution of sodium chloride, successively, dried and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (hexane—ethyl acetate) to give the title compound (950 mg) having the following physical data.

1. customseparated
2. extractionThe aqueous layer was extracted with ethyl acetate
3. washThe combined organic layer was washed with water
4. dry with materiala saturated aqueous solution of sodium chloride, successively, dried
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by column chromatography on silica gel (hexane—ethyl acetate)