Hydrogen Peroxide → 4-Piperidinol, 1-(2-hydroxy-2-methylpropoxy)-2,2,6,6-tetramethyl-

HRID 650429

반응식

OO.[OH:3][CH:4]1[CH2:9][C:8]([CH3:11])([CH3:10])[N:7]([OH:12])[C:6]([CH3:14])([CH3:13])[CH2:5]1.S([O-])([O-])=O.[Na+].[Na+].[C:21]([OH:25])([CH3:24])([CH3:23])[CH3:22]>>[OH:3][CH:4]1[CH2:9][C:8]([CH3:10])([CH3:11])[N:7]([O:12][CH2:22][C:21]([OH:25])([CH3:24])[CH3:23])[C:6]([CH3:14])([CH3:13])[CH2:5]1

참가 물질

반응물 4

HCID 784Hydrogen Peroxide

HCID 53951,4-Dihydroxy-2,2,6,6-tetramethylpiperidine

HCID 6386tert-Butanol

HCID 24437Sodium Sulfite

생성물 1

HCID 68508284-Piperidinol, 1-(2-hydroxy-2-methylpropoxy)-2,2,6,6-tetramethyl-

실험 절차

A solution of 50% aqueous hydrogen peroxide is added to a mixture of 4-hydroxy-1-oxyl-2,2,6,6-tetramethylpiperidine and ferrous chloride tetrahydrate in tert-butyl alcohol at 30-60° C. Excess peroxide is decomposed with aqueous sodium sulfite. The organic layer is concentrated and the crude product is purified by flash chromatography on silica gel to afford a sample of 4-hydroxy-1-(2-hydroxy-2-methylpropoxy)-2,2,6,6-tetramethylpiperidine.

후처리

concentrationThe organic layer is concentrated
customthe crude product is purified by flash chromatography on silica gel

출처 및 근거

ORD 기록: ord-05aae43d3a8a489b8ec0b770e09a4d6b
출처 데이터셋: uspto-grants-2001_08
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US06271377B1

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