反应详情

A solution of N4-cyclohexylmethyl-2-fluoro-5-nitro-N1-phenyl-benzene-1,4-diamine (0.23 g, 0.66 mmol), N-methylpiperazine (0.22 mL, 1.97 mmol) and N,N′-diisopropylethylamine (0.34, 1.97 mmol) in DMF (3.0 mL) was stirred at 100° C. under an inert atmosphere for 16 h. The reaction mixture was transferred to a separatory funnel containing water. The aqueous layer was extracted with EtOAc and the combined organic layers were washed with water, brine and dried over MgSO4. The solution was filtered through diatomaceous earth and the solvent was evaporated. The resulting dark red residue was flash chromatographed (5% MeOH/CH2Cl2) to give N4-cyclohexylmethyl-2-(4-methyl-piperazin-1-yl)-5-nitro-N1-phenyl-benzene-1,4-diamine as a red foam (0.22 g, 80.7% yield). M+, 424

1. customThe reaction mixture was transferred to a separatory funnel
2. extractionThe aqueous layer was extracted with EtOAc
3. washthe combined organic layers were washed with water, brine
4. dry with materialdried over MgSO4
5. filtrationThe solution was filtered through diatomaceous earth
6. customthe solvent was evaporated
7. customchromatographed (5% MeOH/CH2Cl2)