反应详情

温度

50 °C

4-Trimethylsilanylethynyl-pyridin-2-ylamine (7.8 g, 42 mmol) and benzoyl isocynate (12.2 g, 82.9 mmol) are added into DCM (350 mL). The reaction mixture is heated at 50° C. for 16 hrs. Then the solvent is removed and the residue is dissolved in ethanol (350 mL). Potassium carbonate (8.58 g, 62.2 mmol) is added and the mixture is heated at 80° C. for 1 hr. The solvent is removed and the residue is partitioned between water (100 mL) and EtOAc (100 mL). The aqueous layer is separated and extracted with EtOAc (2×100 mL). The organic layers are combined and concentrated to give the crude product. Purification by silica flash column chromatography using 33% EtOAc in hexanes affords 350 mg of the desired product.

1. customThen the solvent is removed
2. dissolutionthe residue is dissolved in ethanol (350 mL)
3. temperaturethe mixture is heated at 80° C. for 1 hr
4. customThe solvent is removed
5. customthe residue is partitioned between water (100 mL) and EtOAc (100 mL)
6. customThe aqueous layer is separated
7. extractionextracted with EtOAc (2×100 mL)
8. concentrationconcentrated
9. customto give the crude product
10. customPurification by silica flash column chromatography