反应详情

2-Methyl-6-Methoxy-1-Tetralone (19 g, 0.1 mole) and pyridine hydrochloride (53.1 g, 0.46 mole) were heated neet, under a nitrogen sweep at about 220° for about 2 hours. The melt was cooled, acidified with 1N HCl and dissolved in ethyl acetate. The organic layers were dried (brine, MgSO4) and concentrated in vacuo. Purification by flash chromatography [gradient 7:1 to 5:1 EtOAc:Hexanes] yielded the title compound as a light yellow solid (14.8 g, 0.084 mole, 84% yield), [Lit. Buchta et al., Ann. 576, 7-19 (1952)].

1. temperatureThe melt was cooled
2. dry with materialThe organic layers were dried (brine, MgSO4)
3. concentrationconcentrated in vacuo
4. customPurification by flash chromatography [gradient 7:1 to 5:1 EtOAc:Hexanes]