反应详情

温度

144 °C

A N,N-dimethylacetamide (30 ml) solution containing 4-nitrofluorobenzene (1.69 g) and trans-1,4-cyclohexanediamine (4.1 g) was stirred at 144° C. for 3 days. After cooling, an aqueous saturated potassium carbonate solution was added to the reaction solution, and the reaction mixture was extracted with ethyl acetate. The extract was dried over anhydrous potassium carbonate, and then, the solvent was removed under reduced pressure. The residue was purified by silica gel flash column chromatography (solvent: chloroform-methanol-ammonia (90:10:1)), and the solvent was removed to obtain trans-N-(4-nitrophenyl)-1,4-cyclohexanediamine (Reference Example 3-41 in Table 5) (2.31 g).

1. temperatureAfter cooling
2. extractionthe reaction mixture was extracted with ethyl acetate
3. dry with materialThe extract was dried over anhydrous potassium carbonate
4. customthe solvent was removed under reduced pressure
5. customThe residue was purified by silica gel flash column chromatography (solvent: chloroform-methanol-ammonia (90:10:1))
6. customthe solvent was removed