反应详情

温度

50 °C

K2CO3 (1.6 g, 11.7 mmol), 2-Fluoro-1-nitro-4-trifluoromethyl-benzene (1.22 g, 5.8 mmol) and trans-4-Aminomethyl-cyclohexanecarboxylic acid methyl ester (1.00 g, 5.84 mmol) were dissolved in DMF (10 ml). The mixture was stirred at 50° C. overnight. The solvent was removed under reduced pressure and the crude product dissolved in DCM (15 ml) and washed with water (20 ml) and then with a solution of citric acid (1M, 5 ml). The organic solution was dried over Na2SO4, filtered and the solvent removed by evaporation to give solid material. This was washed with cyclohexane and then with isopropyl ether and purified by silica column using DCM/cyclo hexane (1:1) as eluent. 1.8 g (yield 86%) of the title compound were isolated.

1. customThe solvent was removed under reduced pressure
2. dissolutionthe crude product dissolved in DCM (15 ml)
3. washwashed with water (20 ml)
4. dry with materialThe organic solution was dried over Na2SO4
5. filtrationfiltered
6. customthe solvent removed by evaporation
7. customto give solid material
8. washThis was washed with cyclohexane
9. customwith isopropyl ether and purified by silica column