反应详情

To a stirred solution of 1,2-bis(4-chlorophenyl)-5-methylpyrrole (1.76 g, 0.006 mol, as obtained in Step-2) in acetonitrile (18 ml) was added a mixture of 1-(3-trifluoromethylphenyl) piperazine hydrochloride (1.55 g, 0.006 mol), 40% formaldehyde (0.45 ml, 0.006 mol) and acetic acid (5.23 ml) drop-wise. After the completion of addition, the reaction mixture was stirred at room temperature for 3-4 hours. The reaction mixture was neutralized with NaOH (20% aq. soln.) and extracted with ethyl acetate (2×100 ml). The combined ethyl acetate extract was washed with water (2×50 ml), brine (1×30 ml), dried over anhydrous sodium sulfate and the solvent evaporated off. The crude product so obtained was purified by column chromatography over silica gel using ethyl acetate hexane (80:10) as eluent to give 2.1 g (66.24%) of the title compound.

1. additionAfter the completion of addition
2. extractionextracted with ethyl acetate (2×100 ml)
3. extractionThe combined ethyl acetate extract
4. washwas washed with water (2×50 ml), brine (1×30 ml)
5. dry with materialdried over anhydrous sodium sulfate
6. customthe solvent evaporated off
7. customThe crude product so obtained
8. customwas purified by column chromatography over silica gel