反应详情

K2CO3 (9.04 g, 65.5 mmol) was added to a solution of 2-Fluoro-4-methoxy-1-nitro-benzene (5.6 g, 32.7 mmol) in DMF (20 ml). The mixture was stirred at room temperature for 30 minutes and then trans-4-Aminomethyl-cyclohexanecarboxylic acid methyl ester (5.60 g, 32.7 mmol) was added. The reaction mixture was heated for 2 hours at 50° C. and then at room temperature overnight. The solvent was removed under reduced pressure and the crude product dissolved in DCM (150 ml) and washed with water (2×150 ml) and then with a solution of citric acid (2×150 ml). The organic solution was dried over Na2SO4, filtered and the solvent removed by evaporation to give 9.6 g of the titled compound.

1. temperatureThe reaction mixture was heated for 2 hours at 50° C.
2. customat room temperature
3. customovernight
4. customThe solvent was removed under reduced pressure
5. dissolutionthe crude product dissolved in DCM (150 ml)
6. washwashed with water (2×150 ml)
7. dry with materialThe organic solution was dried over Na2SO4
8. filtrationfiltered
9. customthe solvent removed by evaporation