反应详情

2-Fluoro-4-methoxybenzaldehyde (6.0 g, 39 mmol) was dissolved in dichloroethane (100 mL) and 1-methylpiperazine (4.5 g, 45 mmol) was added and the solution was stirred at rt for 30 minutes. Sodium triacetoxyborohydride (10 g, 47 mmol) was added in portions and the reaction mixture was stirred at rt over night. Aqueous Na2CO3 (sat.) was added to the reaction and the phases were separated. The aqueous phase were extracted twice with DCM and the combined organic phases were filtered through a phase separator and the solvent was removed by evaporation. There was obtained 9.3 g (100%) of 29A as a brown oil. 1H NMR (500 MHz, CDCl3): δ 2.28 (s, 3H), 2.30-2.70 (bm, 8H), 3.53 (s, 2H), 3.78 (s, 3H), 6.53-6.71 (m, 2H), 7.17-7.27 (m, 1H).

1. stirringthe reaction mixture was stirred at rt over night
2. customthe phases were separated
3. extractionThe aqueous phase were extracted twice with DCM
4. filtrationthe combined organic phases were filtered through a phase separator
5. customthe solvent was removed by evaporation