Hydrogen Peroxide → N-cyclohexyloxy-4-oxo-2,2,6,6-tetramethylpiperidine

HRID 133631

反応式

HRID 133631 の反応式
OO.[OH:3][N:4]1[C:9]([CH3:11])([CH3:10])[CH2:8][C:7](=[O:12])[CH2:6][C:5]1([CH3:14])[CH3:13].CS(O)(=O)=O.[CH2:20]1[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]1>O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Fe+2].CO>[CH:20]1([O:3][N:4]2[C:9]([CH3:10])([CH3:11])[CH2:8][C:7](=[O:12])[CH2:6][C:5]2([CH3:14])[CH3:13])[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]1

参加物

7

反応物 4

HCID 784Hydrogen Peroxide2 回HCID 6395Methanesulfonic AcidHCID 8078CyclohexaneHCID 986421-Hydroxy-2,2,6,6-tetramethyl-4-oxopiperidine

生成物 1

HCID 22019868N-cyclohexyloxy-4-oxo-2,2,6,6-tetramethylpiperidine収率 35%

試薬・触媒・溶媒 2

HCID 62662Ferrous sulfate heptahydrate触媒HCID 887Methanol溶媒

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.

後処理

  1. additionShortly after the addition
  2. concentrationThe reaction mixture is concentrated

出典と根拠

ORDレコード
ord-a53408cb0ce54faa8f117c9a7ef781f0
出典データセット
uspto-grants-2008_06
特許番号
US07390904B2

関連ノート

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