反应详情

4.5 g of 6-(3-bromophenyl)-2-chloromethyl-3(2H)-pyridazinone were heated with 10 ml of N-butyl-N-methylamine at 100°-110° C. on an oil bath for 2 hours. After the reaction mixture had been left to cool, the excess amine was distilled off under reduced pressure. To the resulting residue were added 100 ml of ethyl acetate and the mixture was left to stand overnight. The insolubles were removed by filtration and the filtrate was concentrated by evaporation under reduced pressure to a volume of about 20 ml. 100 ml of hexane and 20 ml of benzene were added to the concentrate and, after adding a small amount of active carbon, the mixture was filtered. The filtrate was concentrated by evaporation under reduced pressure and the residue was dried at 50° C. under a pressure of 13 Pa (0.1 mmHg) for 2 hours, to afford 5.0 g (yield 94%) of the desired Compound No. 13, in the form of a pale brown oil, nD23 =1.5918.

1. waitAfter the reaction mixture had been left
2. temperatureto cool
3. distillationthe excess amine was distilled off under reduced pressure
4. additionTo the resulting residue were added 100 ml of ethyl acetate
5. waitthe mixture was left
6. customThe insolubles were removed by filtration
7. concentrationthe filtrate was concentrated by evaporation under reduced pressure to a volume of about 20 ml
8. addition100 ml of hexane and 20 ml of benzene were added to the
9. concentrationconcentrate
10. additionafter adding a small amount of active carbon
11. filtrationthe mixture was filtered
12. concentrationThe filtrate was concentrated by evaporation under reduced pressure
13. customthe residue was dried at 50° C. under a pressure of 13 Pa (0.1 mmHg) for 2 hours