反应详情

At reflux, a solution of 29.5 g (0.25 mol) of anthranilonitrile in 150 ml of tetrahydrofuran is added dropwise to a suspension comprising 18.2 g (0.75 mmol) of magnesium, 375 ml of a 2 M solution of isobutylmagnesium bromide in tetrahydrofuran and 15 ml of diethyl ether. After 5 h of heating under reflux, 100 ml of water are, at 0° C., added to the reaction mixture, and the pH is adjusted to 6 using hydrochloric acid. The organic phase is washed with water and dried over magnesium sulphate. Concentration under reduced pressure and purification on silica gel (mobile phase: petroleum ether/acetonitrile 95:5) gives 11.0 g (25% of theory) of 1-(2-aminophenyl)-3-methylbutan-1-one of logP (pH 2.3)=2.89.

1. temperatureAt reflux
2. temperatureAfter 5 h of heating
3. temperatureunder reflux
4. customare, at 0° C.
5. additionadded to the reaction mixture
6. washThe organic phase is washed with water
7. dry with materialdried over magnesium sulphate
8. concentrationConcentration
9. customunder reduced pressure and purification on silica gel (mobile phase: petroleum ether/acetonitrile 95:5)