反应详情

To a suspension of hydroxylamine hydrochloride (46.1 g, 0.663 mol) in 1070 mL of acetonitrile was added 2-ethoxy-3-methyl-3,4,5,6-tetrahydrobenzo[h]chromene (140 g, 0.265 mol) from step two. The reaction mixture was heated at reflux under nitrogen with stirring for 16 h. Evaporation of the acetonitrile, followed by vacuum distillation of the product yielded 34.5 g of a crude product that was further purified by silica gel chromatography with 5/95 ethyl acetate/hexane as the eluent, yielding 23.2 g (45%) of 5,6-dihydrobenzo[h]quinoline as a yellow liquid.

1. temperatureThe reaction mixture was heated
2. temperatureat reflux under nitrogen
3. customEvaporation of the acetonitrile
4. distillationfollowed by vacuum distillation of the product
5. customyielded 34.5 g of a crude product that
6. customwas further purified by silica gel chromatography with 5/95 ethyl acetate/hexane as the eluent