反应详情

温度

100 °C

N-(3-tert-Butylphenyl)-4-methylpiperidine-4-carboxamide from step B (0.33 g, 1.07 mmol), 4-chloro-5-methyl-7H-pyrrolo[2,3-d]pyrimidine (0.18 g, 1.07 mmol), N,N-diisopropylethylamine (0.69 g. 5.34 mmol), and isopropanol (7 mL) were combined in a pressure rated sealed tube and heated at 100° C. for 18 hours. The mixture was concentrated and taken up in dichloromethane from which a precipitate (0.18 g) was collected. The solution was chromatographed (SiO2, 0-2% MeOH:CH2Cl2), and the columned material (0.15 g) was combined with the precipitate and dissolved in methanol (15 mL) at 60° C. Water was added (5.0 mL), and the mixture was cooled. The resultant precipitate was filtered, washed with water, and dried to give the title compound in 50% yield.

1. customrated sealed tube
2. concentrationThe mixture was concentrated
3. customwas collected
4. customThe solution was chromatographed (SiO2, 0-2% MeOH:CH2Cl2)
5. dissolutiondissolved in methanol (15 mL) at 60° C
6. additionWater was added (5.0 mL)
7. temperaturethe mixture was cooled
8. filtrationThe resultant precipitate was filtered
9. washwashed with water
10. customdried