反应详情

To a flask mounted with Dean-Stark water removing apparatus (Dean-Stark trap) were added toluene (200 ml), 4-methyl-3-nitroacetophenone (9.77 g, 54.53 mmol), ethylene glycol (4.6 ml) and p-toluenesulfonic acid.monohydrate (0.79 g), and the mixture was heated under reflux for 100 min. The reaction mixture was cooled, washed with diluted aqueous sodium hydroxide solution and saturated brine, and dried over anhydrous magnesium sulfate. The insoluble material was filtered off, and the solution was concentrated under reduced pressure to give a crude brown oil (13.0 g). Using the crude oil and according to the method of Reference Example 61, step B, the title compound (9.89 g, yield 94%) was obtained as a pale-yellow solid.

1. temperatureunder reflux for 100 min
2. temperatureThe reaction mixture was cooled
3. washwashed with diluted aqueous sodium hydroxide solution and saturated brine
4. dry with materialdried over anhydrous magnesium sulfate
5. filtrationThe insoluble material was filtered off
6. concentrationthe solution was concentrated under reduced pressure
7. customto give a crude brown oil (13.0 g)