反应详情

温度

122 °C

To a stirred solution of 5-bromo-6-(2-furyl)pyrazin-2-amine (Preparation 2, 1.5 g, 6.3 mmol) in a mixture of DMF (16 mL) and water (4 mL) was added butyl vinyl ether (4.10 mL, 31.5 mmol), potassium acetate (3.80 mL, 7.56 mmol), 1,3-bis-(diphenylphosphino)propane (0.172 g, 0.416 mmol) and palladium(II) acetate (42.0 mg, 0.189 mmol)1. The mixture was subjected to three cycles of evacuation-backfilling with argon and heated at 122° C. under microwave irradiation. After 4 h, the mixture was cooled to room temperature and hydrolyzed by adding of HCl 2N (30 mL) for 30 min. The mixture was then neutralized with a saturated solution of potassium carbonate and diluted with dichloromethane. The organic layer was separated, dried (Na2SO4) and evaporated. The residue was purified by silica gel flash chromatography (2% methanol in dichloromethane). Concentration in vacuo of the product-rich fractions provided the titled compound as a pale-yellow solid (0.77 g, 60%). 1K. S. A. Vallin, M. Larhed, A. Hallberg, J. Org. Chem., 2001, 66, 4340.

1. temperaturethe mixture was cooled to room temperature
2. customThe organic layer was separated
3. dry with materialdried (Na2SO4)
4. customevaporated
5. customThe residue was purified by silica gel flash chromatography (2% methanol in dichloromethane)
6. concentrationConcentration in vacuo of the product-rich fractions