反应详情

15.45 g (60.2 mmol) of tert-butyl (6-chloro-3-formylpyridin-2-yl)carbamate (Example 2A) were initially charged in 750 ml of ethanol and admixed with a solution of 225 ml of water and 9.38 g (120.4 mmol) of sodium acetate and stirred for 5 min. A solution of 225 ml of water and 8.36 g (114.4 mmol) of hydroxylamine hydrochloride was added and the mixture was stirred at RT for 4 h. At 20° C., the reaction mixture was concentrated on a rotary evaporator. The residue was taken up in ethyl acetate and washed twice with saturated sodium hydrogencarbonate solution and once with saturated sodium chloride solution. The organic phase was removed, dried over magnesium sulphate and concentrated at 20° C. on a rotary evaporator. 15.5 g (80% of theory) of the product were obtained in solid form.

1. stirringthe mixture was stirred at RT for 4 h
2. concentrationAt 20° C., the reaction mixture was concentrated on a rotary evaporator
3. washwashed twice with saturated sodium hydrogencarbonate solution and once with saturated sodium chloride solution
4. customThe organic phase was removed
5. dry with materialdried over magnesium sulphate
6. concentrationconcentrated at 20° C. on a rotary evaporator
7. custom15.5 g (80% of theory) of the product were obtained in solid form