反応 #220813

反応方程式

hydrogen peroxide

1-oxyl-2,2,6,6-tetramethylpiperid-4-one

methanesulfonic acid

cyclohexane

hydrogen peroxide

→

title compound

収率 35.0%

1-Cyclohexyloxy-2,2,6,6-tetramethylpiperidin-4-one

収率 35.0%

溶媒

methanol

反応条件

後処理

1. 1
   workup.ADDITIONShortly after the addition
2. 2
   濃縮The reaction mixture is concentrated

実験手順

A solution of 20.1 g (0.295 mol) of 50% aqueous hydrogen peroxide is added over 6 hours at 60° C. to a mixture of 8.51 g (50.0 mmol) of 1-oxyl-2,2,6,6-tetramethylpiperid-4-one, 0.70 g (2.5 mmol) of iron(II) sulfate heptahydrate, 0.3 ml (5 mmol) of methanesulfonic acid, 11 ml of cyclohexane, and 90 ml of methanol. Shortly after the addition is completed, the reaction mixture tests negative for hydrogen peroxide. The reaction mixture is concentrated to afford 4.4 g (35% yield) of the title compound, isolated as a yellow oil. Structure is confirmed by mass spectrometry and NMR analysis.

出典