反应详情

A stirred mixture of ethyl{trans-4-[(ethylamino)methyl]cyclohexyl}acetate (Intermediate 7; 130 mg; 0.57 mmol), 2-fluoro-5-(trifluoromethyl)benzaldehyde (100 mg; 0.52 mmol) and potassium carbonate (215 mg; 1.56 mmol) in toluene (4 mL) was heated at reflux for 14 h. The reaction was washed with H2O and sat. KHSO4 (10 mL each) and the aqueous layers were re-extracted with toluene (10 mL). The combined organic layers were washed with brine (10 mL), dried (MgSO4), filtered and concentrated in vacuo to afford ethyl [trans-4-({ethyl[2-formyl-4-(trifluoromethyl)phenyl]amino}methyl)cyclohexyl]acetate as a yellow oil. LCMS=400.2 (M+1)+.

1. temperaturewas heated
2. temperatureat reflux for 14 h
3. washThe reaction was washed with H2O and sat. KHSO4 (10 mL each)
4. extractionthe aqueous layers were re-extracted with toluene (10 mL)
5. washThe combined organic layers were washed with brine (10 mL)
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. concentrationconcentrated in vacuo