反应详情

温度

2 °C

A solution of 2 g 2,4-dichloro-6-fluoro-7-isothiocyanatobenzothiazole in 10 ml dichloromethane was added, dropwise, at 0° C., to a suspension of 1.1 g 2-amino-4,4-dimethylpyrroline hydrochloride in 20 ml dichloromethane. A solution of 0.3 g sodium hydroxide and 6 ml water was added, dropwise, at 2° C. to this mixture which was stirred for 3 hours, whereby the temperature rose to 20° C. The mixture was cooled to -10° C. and a solution of 1 g bromine in 10 ml dichloromethane was added, dropwise, slowly and the mixture stirred for I hour whereby the temperature rose to 10° C. The solution was washed with water and with dilute caustic soda, dried over magnesium sulfate and concentrated. The residue was recrystallised from diisopropyl ether. Yield: 1.5 g=53% of theory m.p.: 134°-136° C.

1. customrose to 20° C
2. temperatureThe mixture was cooled to -10° C.
3. stirringdropwise, slowly and the mixture stirred for I hour whereby the temperature
4. customrose to 10° C
5. washThe solution was washed with water and with dilute caustic soda
6. dry with materialdried over magnesium sulfate
7. concentrationconcentrated
8. customThe residue was recrystallised from diisopropyl ether