反应详情

温度

0 °C

11.15 g (53.6 mmol) of 2-amino-6-chloropyridine-3-carbaldehyde oxime hydrochloride (Example 4A) were initially charged in dioxane, admixed with 13 ml (161 mmol) of pyridine and cooled to 0° C. 8.3 ml (58.95 mmol) of trifluoroacetic anhydride were added, and the reaction was warmed to RT and then stirred at 60° C. for 2 h. The reaction mixture was taken up in a mixture of ethyl acetate and sodium hydrogencarbonate solution. The organic phase was washed with saturated aqueous sodium chloride solution, dried over magnesium sulphate and concentrated on a rotary evaporator. The residue was suspended in 3:1 dichloromethane:diethyl ether, and the solids were filtered off with suction and dried. 5.56 g (66% of theory) of the product were obtained in solid form.

1. temperaturethe reaction was warmed to RT
2. washThe organic phase was washed with saturated aqueous sodium chloride solution
3. dry with materialdried over magnesium sulphate
4. concentrationconcentrated on a rotary evaporator
5. filtrationdiethyl ether, and the solids were filtered off with suction
6. customdried
7. custom5.56 g (66% of theory) of the product were obtained in solid form