反应详情

温度

110 °C

2-Chloropyrimidine (0.72 g, 6.3 mmol) and N-(4-aminobenzoyl)-L-glutamic acid diethyl ester (2.04 g, 6.3 mmol, 1 equiv.) were dissolved in DMF (4 mL) and the resulting mixture was heated to 110° C. for 3 hrs. Reaction was complete as determined by TLC. The mixture was cooled to room temperature and partitioned between ethyl acetate and water. The organic phase was washed with brine, dried over MgSO4, and concentrated by rotavap. The residue was purified by column chromatography (silica gel, 50% EtOAc/hexane) to afford 1.75 g of desired product 2-[4-(pyrimidin-2-ylamino)-benzoylamino]-pentanedioic acid diethyl ester in 69% yield. MS (ESI) m/z 399.

1. customReaction
2. temperatureThe mixture was cooled to room temperature
3. custompartitioned between ethyl acetate and water
4. washThe organic phase was washed with brine
5. dry with materialdried over MgSO4
6. concentrationconcentrated by rotavap
7. customThe residue was purified by column chromatography (silica gel, 50% EtOAc/hexane)