反应详情

温度

80 °C

A mixture of 4-(2-bromo-5-fluorophenoxy)piperidine-1-carbonitrile (1.6 g, 5.3 mmol), hydroxylamine hydrochloride (1.1 g, 16.1 mmol) and Na2CO3 (2.3 g, 92 mmol) in EtOH/water 4:1 (26 ml) was heated at 80° C. for 1 h. The solvent was evaporated. The residue was acidified with 6N HCl and washed with Et2O (2×10 mL). The aqueous layer was made basic with solid Na2CO3 and extracted with EtOAc (3×20 mL). The combined organic fractions were dried over Na2SO4 and the solvent was evaporated under reduced pressure to give the title compound as a foam which was used in the next step without further purification. MS: m/z 332, 334 (MH+).

1. customThe solvent was evaporated
2. washwashed with Et2O (2×10 mL)
3. extractionextracted with EtOAc (3×20 mL)
4. dry with materialThe combined organic fractions were dried over Na2SO4
5. customthe solvent was evaporated under reduced pressure