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

HRID 133631

반응식

HRID 133631 반응식
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

참가 물질

7

반응물 4

HCID 784Hydrogen Peroxide2회HCID 6395Methanesulfonic AcidHCID 8078CyclohexaneHCID 986421-Hydroxy-2,2,6,6-tetramethyl-4-oxopiperidine

생성물 1

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

시약·촉매·용매 2

HCID 62662Ferrous sulfate heptahydrate촉매HCID 887Methanol용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-a53408cb0ce54faa8f117c9a7ef781f0
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07390904B2

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