反应详情

2-Fluoro-6-(4-methyl-1-piperazinyl)pyridine-3-carboxaldehyde acetylhydrazone (2.30 g, 8.23 mmole) was warmed at 90° C. in 10 mL of methylhydrazine. After 30 minutes the reaction mixture was concentrated under reduced pressure and the resulting solid triturated with water. The product was filtered off and the aqueous filtrate was extracted three times with CH2Cl2. The CH2Cl2 was evaporated and the residual product was combined with the product that had been previously filtered off and the two were recrystallized together from pentane, giving 1.37 g (72%), mp 106°-107° C.

1. concentrationAfter 30 minutes the reaction mixture was concentrated under reduced pressure
2. customthe resulting solid triturated with water
3. filtrationThe product was filtered off
4. extractionthe aqueous filtrate was extracted three times with CH2Cl2
5. customThe CH2Cl2 was evaporated
6. filtrationhad been previously filtered off
7. customthe two were recrystallized together from pentane
8. customgiving 1.37 g (72%), mp 106°-107° C.