反应详情

To a solution of 6-oxo-piperidine-3-carboxylic acid (XLIX) (0.22 g, 1.5 mmol) in dry DMF (10 ml) was added HBTU (1.13 g, 2.98 mmol) and DIPEA (0.40 ml, 2.3 mmol) under ice cooled condition, and then it was allowed to stir at room temperature for 45 minutes. To this reaction mixture was added 6-(2-methoxy-phenyl)-pyrimidin-4-ylamine (XXIV) (0.30 g, 1.5 mmol) in dry DMF dropwise at ice bath temperature. The reaction mixture was then heated for 4 hours at 120° C. After completion of the reaction, it was cooled and DMF was evaporated completely. The residue was dissolved in ethyl acetate (30 ml), washed with water (2×15 ml) and brine, dried over anhydrous sodium sulfate and evaporated under reduced pressure. Final purification was achieved by flash column chromatography using silica gel (10% methanol/dichloromethane) to give 6-oxo-piperidine-3-carboxylic acid [6-(2-methoxy-phenyl)-pyrimidin-4-yl]amide. Yield: 78.2 mg, 17%.

1. temperatureThe reaction mixture was then heated for 4 hours at 120° C
2. customAfter completion of the reaction, it
3. temperaturewas cooled
4. customDMF was evaporated completely
5. dissolutionThe residue was dissolved in ethyl acetate (30 ml)
6. washwashed with water (2×15 ml) and brine
7. dry with materialdried over anhydrous sodium sulfate
8. customevaporated under reduced pressure
9. customFinal purification