反应详情

温度

70 °C

4-Chloropyrido[3,4-d]pyrimidine (0.10 g, 0.60 mmol), 6-chloroindoline (0.10 g, 0.66 mmol) and pyridine (0.14 g, 1.81 mmol) were combined in DMF (1 mL) and heated at 70° C. for 3 hours. The reaction was cooled to room temperature and then added to methylene chloride (150 mL). The organic layer was washed with saturated sodium carbonate and water and then dried over sodium sulfate. The solvent was removed by rotary evaporation and the residue purified by column chromatography (silica gel, 9/2/1—CH2Cl2/hexanes/methanol) to give the title product as a pale yellow residue (0.048 g, 28%). MP 194-6° C.; LCMS: 283 (MH+).

1. temperatureThe reaction was cooled to room temperature
2. washThe organic layer was washed with saturated sodium carbonate and water
3. dry with materialdried over sodium sulfate
4. customThe solvent was removed by rotary evaporation
5. customthe residue purified by column chromatography (silica gel, 9/2/1—CH2Cl2/hexanes/methanol)