反应详情

温度

0 °C

A suspension of 2,4-dichloro-6-methoxybenzaldehyde oxime (2.24 mmol) in 3 mL AcOH was cooled to 0° C. and zinc dust (8.53 mmol) was added. The reaction mixture was stirred at RT for 2 h. It was filtered over a pad of celite and washed with EtOAc and MeOH. The filtrate was conc. and redissolved in water (pH 4 with 2N HCl solution). It was washed once with EtOAc, the ageous phase was basified with 1M NaOH solution, extracted 3 times with EtOAc and DCM. The comb. org. layers were dried over MgSO4 and conc. in vacuo to give the desired product as yellow solid.

1. filtrationIt was filtered over a pad of celite
2. washwashed with EtOAc and MeOH
3. dissolutionredissolved in water (pH 4 with 2N HCl solution)
4. washIt was washed once with EtOAc
5. extractionextracted 3 times with EtOAc and DCM
6. dry with materiallayers were dried over MgSO4 and conc. in vacuo