反应详情

In a 100 ml two-necked flask, 1.55 g (2.1 mmol) of dichlorobis(triphenylphosphine)nickel(II), 452 mg (6.95 mmol) of zinc and 2.23 g (6.95 mmol) of tetrabutylammonium bromide are solubilized in 40 ml of freshly distilled DMF. After degassing, the solution is stirred at ambient temperature for 30 min (the green starting solution turns brown). 1 g (6.95 mmol) of 3-chloro-6-methoxypyridazine 14 is added to this solution, and the reaction mixture is heated at 55° C. for 8 hours. After the solvent has been evaporated off under reduced pressure, the residue is taken up in a saturated solution of ammonium chloride, the suspension is extracted with 4×40 ml of dichloromethane and the organic phase is dried over MgSO4 and then concentrated under reduced pressure. The reaction crude is chromatographed on silica gel (eluent:ethyl acetate/petroleum ether=4/6), to give the bipyridazine 15 with a yield of 96%.

1. customAfter degassing
2. temperaturethe reaction mixture is heated at 55° C. for 8 hours
3. customAfter the solvent has been evaporated off under reduced pressure
4. extractionthe suspension is extracted with 4×40 ml of dichloromethane
5. dry with materialthe organic phase is dried over MgSO4
6. concentrationconcentrated under reduced pressure
7. customThe reaction crude
8. customis chromatographed on silica gel (eluent:ethyl acetate/petroleum ether=4/6)