反应详情

Dissolve 1-(4-bromo-2-methoxy-phenyl)-piperazine (7.0 g, 25.8 mmol) and acetic acid (5.9 mL, 103.2 mmol) in methanol (500 mL) and add aqueous formaldehyde (37%, 5.3 mL). After 5 min, add sodium cyanoborohydride (4.05 g, 64.5 mmol) and stir the mixture at room temperature overnight. Concentrate the reaction mixture in vacuo and partition between dichloromethane (200 mL) and 1 N sodium hydroxide (200 mL). Separate the organic portion and extract the aqueous portion with dichloromethane (2×100 mL). Dry the combined organics (Na2SO4), filter, and concentrate in vacuo to afford 7.1 g (96%) of the title compound. MS/ES m/z (79Br) 285.0 [M+H]−.

1. concentrationConcentrate the reaction mixture in vacuo
2. custompartition between dichloromethane (200 mL) and 1 N sodium hydroxide (200 mL)
3. customSeparate the organic portion
4. extractionextract the aqueous portion with dichloromethane (2×100 mL)
5. dry with materialDry the combined organics (Na2SO4)
6. filtrationfilter
7. concentrationconcentrate in vacuo