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Hydrogen Peroxide → alpha-(2,4-difluorophenyl)-N-[dimethyl(methoxymethyl) methyl]nitrone

HRID 636735
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HRID 636735 반응식
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[CH2:9][NH:10][C:11]([CH3:16])([CH3:15])[CH2:12][O:13][CH3:14].[OH:17]O.[Na+].[Cl-]>CO>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[CH:9]=[N+:10]([C:11]([CH3:16])([CH3:15])[CH2:12][O:13][CH3:14])[O-:17]
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참가 물질

5

반응물 3

HCID 784Hydrogen PeroxideHCID 5234Sodium ChlorideHCID 21255704N-(2,4-difluorophenylmethyl)-N-[dimethyl(methoxymethyl)methyl]amine

생성물 1

HCID 72602289alpha-(2,4-difluorophenyl)-N-[dimethyl(methoxymethyl) methyl]nitrone수율 51%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of N-(2,4-difluorophenylmethyl)-N-[dimethyl(methoxymethyl)methyl]amine obtained in Example 14 (378.8 mg, 1.65 mmol) and Na2WO4 2H2O (84.3 mg, 0.256 mmol) in methanol (5 ml) was cooled to 0° C. in ice-water bath. To the mixture was added dropwise 31% H2O2 aqueous solution (439.3 mg, 4.00 mmol). After addition the mixture was gradually warmed to room temperature and stirred for 15 hours. The mixture was added to sat. NaCl aqueous solution and extracted three times with ethyl acetate and dried over MgSO4. The mixture was concentrated and purified by silica gel chromatography (toluene/ethyl acetate=5/1) to give the title compound (204.8 mg; 51%).

후처리

  1. additionAfter addition the mixture
  2. extractionextracted three times with ethyl acetate
  3. dry with materialdried over MgSO4
  4. concentrationThe mixture was concentrated
  5. custompurified by silica gel chromatography (toluene/ethyl acetate=5/1)

출처 및 근거

ORD 기록
ord-4d225aabeb784a0ca64a287642cac08b
출처 데이터셋
uspto-grants-2001_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06194461B1

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