反应详情

温度

100 °C

To a clean, dry, nitrogen-purged 1.0 L reactor were charged methyl-(4-methyl-piperidin-3-yl)-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)-amine (32.0 g, 0.130 mol), toluene (160 ml), ethyl cyanoacetate (88.53 g, 0.783 mol) and triethyl amine (26.4 g, 0.261 mol). The reaction was heated to 100° C. and held for 24 hours. The reaction was washed with water (160 ml). The organic layer concentrated to a volume of 10 ml and water (20 ml) was added. The residual toluene was removed by distillation and the mixture was cooled to room temperature. Acetone (224 ml) was added followed by citric acid (27.57 g, 0.144 mol) in water (76 ml). The resulting slurry was stirred for 7 hours. The solids were isolate by filtration, washed with acetone (96 ml), and dried under vacuum to afford 42.85 g (65.3%) of the title compound.

1. customTo a clean, dry
2. customnitrogen-purged 1.0 L reactor
3. washThe reaction was washed with water (160 ml)
4. concentrationThe organic layer concentrated to a volume of 10 ml and water (20 ml)
5. additionwas added
6. customThe residual toluene was removed by distillation
7. temperaturethe mixture was cooled to room temperature
8. additionAcetone (224 ml) was added
9. customThe solids were isolate by filtration
10. washwashed with acetone (96 ml)
11. customdried under vacuum