反应详情

THF (45 ml) solution of 3-(phenylthio)acryloyl chloride (3.03 g) was added to THF (45 ml) solution of triethylamine (2.09 ml) under ice-cooling. 3-methylaniline (1.62 g) was added to the mixture under ice-cooling and stirred at room temperature for ten hours. The reaction solution was concentrated under reduced pressure. Ice cooled 1N hydrochloric acid (40 ml) and ethyl acetate (200 ml) were added to the residue and separated to two layer. The organic layer was washed with aqueous saturated sodium chloride solution (40 ml) twice, dried over anhydrous magnesium sulfate, filtered off inorganic salt and concentrated under reduced pressure to obtain N-(3-methylphenyl)-3-(phenylthio)acrylamide (3.46 g).

1. temperaturecooling
2. temperaturecooling
3. concentrationThe reaction solution was concentrated under reduced pressure
4. temperatureIce cooled 1N hydrochloric acid (40 ml) and ethyl acetate (200 ml)
5. additionwere added to the residue
6. customseparated to two layer
7. washThe organic layer was washed with aqueous saturated sodium chloride solution (40 ml) twice
8. dry with materialdried over anhydrous magnesium sulfate
9. filtrationfiltered off inorganic salt
10. concentrationconcentrated under reduced pressure