反应详情

温度

45 °C

In a 50 mL round-bottomed flask was added tert-butyl 4-(4-(azetidine-3-carboxamido)phenyl)piperidine-1-carboxylate (918 mg, 2.55 mmol) and diisopropylethylamine (0.558 ml, 3.19 mmol) in ethanol (10.6 ml). 3,6-dichloropyridazine (317 mg, 2.128 mmol) was added as a solid in a single portion. The reaction was stirred overnight at 45° C.; and the reaction was cooled and concentrated. Dichloromethane and water were added and the layers were separated. The aqueous layer was extracted three times with dichloromethane and the combined organics were dried with magnesium sulfate, filtered and concentrated by rotary evaporation. The residue was purified by regular phase flash column chromatography to give the title compound.

1. temperatureand the reaction was cooled
2. concentrationconcentrated
3. additionDichloromethane and water were added
4. customthe layers were separated
5. extractionThe aqueous layer was extracted three times with dichloromethane
6. dry with materialthe combined organics were dried with magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated by rotary evaporation
9. customThe residue was purified by regular phase flash column chromatography