反应详情

A solution of 12.6 g (42.2 mmol) of N-n-butyl-N-[1-(2-hydroxyethyl)-2,2,6,6-tetramethylpiperidin-4-yl]acetamide [Example 1bη2] in 180 ml of 2N hydrochloric acid is refluxed for 48 hours. The reaction mixture is then cooled 0°-5° C. and, after addition of 40 ml of 30% sodium hydroxide solution, extracted twice with toluene. The organic phases are washed with water, combined, dried over sodium sulfate and concentrated on a vacuum rotary evaporator. Chromatography of the residue over silica gel with the solvent system ethyl acetate/ethanol/triethylamine=50:2:1 gives 8.1 g (68%) of 2-(4-n-butylamino-2,2,6,6-tetramethylpiperidin-1-yl) ethanol (208) in the form of a white powder, m.p. 106°-111° C.

1. temperatureThe reaction mixture is then cooled 0°-5° C.
2. extractionextracted twice with toluene
3. washThe organic phases are washed with water
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated on a vacuum rotary evaporator