反应详情

The title compound is synthesized according to general procedure GP3 starting from 2.0 g (7.8 mmol) 5-(4-Chloro-2-ethyl-pyridin-3-ylethynyl)-pyridin-2-ylamine (A-30) using 2.5 g (11.6 mmol) 3-chloro-4-methoxycarbonylphenyl boronic acid, 335 mg (0.39 mmol) Pd2(dba)3, 555 mg (1.2 mmol) X-Phos and 2.7 g (11.6 mmol) K3PO4 in a mixture of 100 mL DME and 20 mL water. The reaction mixture is stiffed under reflux for 4 days. The DME is removed under reduced pressure and the aqueous is extracted with ethyl acetate. The organic phase is dried over Na2SO4, filtered and the solvent removed under vacuum. The product is purified by chromatography on silica gel using an DCM/MeOH-gradient. Yield: 0.59 g (19%).

1. temperatureunder reflux for 4 days
2. customThe DME is removed under reduced pressure
3. extractionthe aqueous is extracted with ethyl acetate
4. dry with materialThe organic phase is dried over Na2SO4
5. filtrationfiltered
6. customthe solvent removed under vacuum
7. customThe product is purified by chromatography on silica gel using an DCM/MeOH-gradient