反应详情

To a 5-mL microwave safe vial was added potassium fluoride (0.151 g, 2.59 mmol), palladium (II) acetate (0.012 g, 0.052 mmol), 2-(4-(difluoromethoxy)phenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (0.28 g, 1.037 mmol), methyl 6-amino-2-chloro-5-methoxypyrimidine-4-carboxylate (0.226 g, 1.037 mmol), and 3,3′,3″-phosphinetriyltribenzenesulfonate (0.052 g, 0.104 mmol). A mixture of water (1 mL) and acetonitrile (2 mL) was added and the reaction was capped and placed in a Biotage Initiator™ microwave reactor for 6 min at 160° C., with external IR-sensor temperature monitoring from the side of the vessel. Upon cooling to room temperature, the reaction mixture was diluted with EtOAc (50 mL) and water (50 mL). An additional extraction using CH2Cl2 (50 mL) was combined with the EtOAc and dried over of Na2SO4 (50 g) after the CH2Cl2 layer was filtered through cotton plug. The combined organics were concentrated on a rotary evaporator and the residue was purified using a Teledyne ISCO purification system with a gradient eluent system of CH2Cl2 and EtOAc to yield the title compound as a tan solid (134.4 mg).

1. additionwas added
2. customthe reaction was capped
3. extractionAn additional extraction
4. dry with materialdried over of Na2SO4 (50 g) after the CH2Cl2 layer
5. filtrationwas filtered through cotton plug
6. concentrationThe combined organics were concentrated on a rotary evaporator
7. customthe residue was purified
8. customa Teledyne ISCO purification system with a gradient eluent system of CH2Cl2 and EtOAc