反应详情

To a mixture of 4-aminocyclohexanol (3.51 g, 23.15 mmol) and K2CO3 (12.80 g, 93 mmol) in acetonitrile (100 mL) was added benzylbromide (5.64 mL, 47.5 mmol) and the mixture was stirred at reflux for 17 hr. The crude mixture was concentrated in vacuo and the resulting residue was dissolved in water and EtOAc. The separated aqueous layer was extracted with EtOAc (2ט100 mL). The combined organic layers were washed with brine, dried over Na2SO4, filtered off and concentrated in vacuo providing crude 4-(dibenzylamino)cyclohexanol as a viscous oil, which was directly used in the next step without further purification. Yield: 6.12 g. LCMS (m/z): 296.1 [M+H]+; Retention time=0.59 min.

1. temperatureat reflux for 17 hr
2. concentrationThe crude mixture was concentrated in vacuo
3. dissolutionthe resulting residue was dissolved in water
4. extractionThe separated aqueous layer was extracted with EtOAc (2ט100 mL)
5. washThe combined organic layers were washed with brine
6. dry with materialdried over Na2SO4
7. filtrationfiltered off
8. concentrationconcentrated in vacuo