反应详情

温度

80 °C

Add hydroxylamine hydrochloride (0.379 g, 5.458 mmol) and a solution of NaOH (0.327 g, 8.187 mmol) in water (2 mL) to a solution of 4-(2-pyridyl)-benzaldehyde (0.5 g, 2.729 mmol) in ethanol (10 mL). Heat the mixture at 80° C. for 2 h. Cool to ambient temperature and remove the solvent in vacuo. Partition the residue between EtOAc and water. Separate and day the organic phase over Na2SO4, filter and concentrate in vacuo. Purify by chromatography on silica gel eluting with hexane/EtOAc (1:0 and 4:1) to obtain the desired intermediate (311 mg, 58%). GC-MS m/z: 198 (M+).

1. temperatureCool to ambient temperature
2. customremove the solvent in vacuo
3. customPartition the residue between EtOAc and water
4. customSeparate and day the organic phase over Na2SO4
5. filtrationfilter
6. concentrationconcentrate in vacuo
7. customPurify by chromatography on silica gel eluting with hexane/EtOAc (1:0 and 4:1)