反应详情

The Grignard solution was subsequently added dropwise to a solution of 120 g (0.57 mol) of 2-bromonaphthalene and 3.5 g of bis(triphenylphosphine)nickel chloride in 800 cm3 of toluene at such a rate that the internal temperature did not exceed 50° C. Subsequently, the mixture was heated under reflux for a further 3 hours, admixed with 500 ml of 10% strength aqueous HCl, the phases were separated and the organic phase was freed of solvent under reduced pressure. Filtration through silica gel (hexane) gave 107 g (87%) of 13 as a colorless oil. 1H-NMR (100 MHz, CDCl3): 7.0-7.9 (m, 11H, arom. H), 1.9 (s, 3H, CH3).

1. customdid not exceed 50° C
2. temperatureSubsequently, the mixture was heated
3. temperatureunder reflux for a further 3 hours
4. customthe phases were separated
5. filtrationFiltration through silica gel (hexane)