反应详情

32.1 g (0.25 mol) of o-chlorophenol were slowly added dropwise under nitrogen to a mixture of 20.5 g (0.5 mol) of 95% by weight pure crystalline sodium amide and 750 ml of diethylamine. The reaction mixture was refluxed under nitrogen for 72 h with stirring. The workup comprised hydrolysis with 100 ml of saturated aqueous ammonium chloride solution, distillative removal of excess diethylamine, neutralization with dilute hydrochloric acid up to a pH of 7.5, extraction of the residue with a total of 600 ml of methylene chloride, drying over sodium sulfate and concentrating of the organic phase. Thereafter the crude oil thus obtained (46.3 g) was distilled, which yielded 31.5 g (76%) of 3-diethylaminophenol (purity>96% (GC)).

1. temperatureThe reaction mixture was refluxed under nitrogen for 72 h
2. customhydrolysis
3. customwith 100 ml of saturated aqueous ammonium chloride solution, distillative removal of excess diethylamine, neutralization with dilute hydrochloric acid
4. extractionup to a pH of 7.5, extraction of the residue with a total of 600 ml of methylene chloride
5. dry with materialdrying over sodium sulfate
6. concentrationconcentrating of the organic phase
7. customThereafter the crude oil thus obtained (46.3 g)
8. distillationwas distilled