反应详情

To a round-bottom flask was added the crude N1,N1′-([1,1′-biphenyl]-3,5-diylbis(methylene))bis(N3-(3-aminopropyl)propane-1,3-diamine) (3.5 g, 8.0 mmol) and MeOH (50 mL). To the solution was added isobutyraldehyde (1.15 g, 15.9 mmol) and the reaction mixture was stirred at rt for 24 h. Sodium borohydride (1.2 g, 31.9 mmol) was added and the reaction mixture was stirred for 1 h. The reaction mixture was concentrated under reduced pressure to afford a white solid. Aq. NaOH (10%, 200 mL) and EtOAc (200 mL) were added, and the mixture was stirred for 1 h. The layers were separated and the aqueous layer was extracted with EtOAc (200 mL). The combined organics were dried over Na2SO4, filtered, and concentrated under reduced pressure to afford the desired product as a clear oil which was used without further purification.

1. stirringthe reaction mixture was stirred for 1 h
2. concentrationThe reaction mixture was concentrated under reduced pressure
3. customto afford a white solid
4. stirringthe mixture was stirred for 1 h
5. customThe layers were separated
6. extractionthe aqueous layer was extracted with EtOAc (200 mL)
7. dry with materialThe combined organics were dried over Na2SO4
8. filtrationfiltered
9. concentrationconcentrated under reduced pressure