反应详情

To a 50 ml volume three-necked flask, 1-(4-fluorophenyl)-2-methylsulfonylethan-1-one (7-2-3) (5.0 g), methylhydrazine (14-a) (1.2 g), and ethanol (17.1 ml) were added under a nitrogen atmosphere, and heated to reflux for 4 hours. After the mixture was cooled, the precipitated solid was removed by filtration. The filtrate was concentrated under reduced pressure. To the residue was added hot hexane to be dissolved. The mixture was left to cool. Then, the precipitated crystals were collected by filtration, washed, and dried under reduced pressure. The crystal was purified by recrystallization (methanol) to give 1.8 g of 1-[1-(4-fluorophenyl)-2-methylsulfonylethylidene]-2-methylhydrazine (5-2-4).

1. temperatureheated
2. temperatureto reflux for 4 hours
3. temperatureAfter the mixture was cooled
4. customthe precipitated solid was removed by filtration
5. concentrationThe filtrate was concentrated under reduced pressure
6. additionTo the residue was added hot hexane
7. dissolutionto be dissolved
8. waitThe mixture was left
9. temperatureto cool
10. filtrationThen, the precipitated crystals were collected by filtration
11. washwashed
12. customdried under reduced pressure
13. customThe crystal was purified by recrystallization (methanol)