反应详情

To a flask fitted with reflux condenser and stirrer containing 4-butoxy-2,6-dimethylazobenzene (53.4 g, 0.189 mole) was added 50% aqueous ethanol (480 ml). The mixture was heated close to boiling with stirring and sodium hydrosulfite (Na2S2O4, 121.4 g., 697 mole) was added in small portions over a period of 30 min. The mixture was refluxed for 75 min. Most of the alcohol was distilled off and the oily amine layer formed in the operation was taken up in ether. The aqueous phase was made alkaline with sodium hydroxide and was extracted with ether. All the combined ether extracts were dried (Na2SO4), were filtered, and all low-boiling components were evaporated at reduced pressure (solvent and aniline), after which the residue was fractionated by distillation in vacuo. The fraction boiling at 105°-108° (0.1 mm Hg) was collected. Yield: (63%); nD25 =1.5337. [Cf. E. Honkanen, Ann. Acad. Sci. Fennicae, Ser. AII, 99 (1960)].

1. customTo a flask fitted
2. temperaturewith reflux condenser and stirrer
3. temperatureThe mixture was heated
4. customclose
5. temperatureThe mixture was refluxed for 75 min
6. distillationMost of the alcohol was distilled off