反应详情

1-Methylpiperazine (42 μL), N,N-diisopropylethylamine (66 μL), and (1-cyano-2-ethoxy-2-oxoethylidene aminooxy)dimethylamino-morpholino-carbenium hexafluorophosphate (187 mg) were added to a mixture of {2-cyano-4-[4-ethoxy-3-(trifluoromethyl)phenyl]-7H-pyrrolo[2,3-d]pyrimidin-7-yl}acetic acid (100 mg) and DMF (4 mL) at room temperature, and the mixture was stirred at the same temperature for 2 hours. After water was added to the reaction mixture, the precipitate was collected by filtration, and washed with water. After the obtained solid was dissolved in CHCl3, the solution was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (CHCl3:MeOH=100:0 to 50:50), whereby 4-[4-ethoxy-3-(trifluoromethyl)phenyl]-7-[2-(4-methylpiperazin-1-yl)-2-oxoethyl]-7H-pyrrolo[2,3-d]pyrimidine-2-carbonitrile (82 mg) was obtained as a white solid.

1. filtrationthe precipitate was collected by filtration
2. washwashed with water
3. dissolutionAfter the obtained solid was dissolved in CHCl3
4. concentrationthe solution was concentrated under reduced pressure
5. customThe residue was purified by silica gel column chromatography (CHCl3:MeOH=100:0 to 50:50)