Hydrogen Peroxide → 4-(3-(tert-Butoxycarbonyl)phenyl)-3-methylpyridine 1-oxide

HRID 39453

반응식

HRID 39453 반응식
[CH3:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[C:8]1[CH:9]=[C:10]([CH:18]=[CH:19][CH:20]=1)[C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12].[OH:21]O>ClCCl.C[Re](=O)(=O)=O>[C:14]([O:13][C:11]([C:10]1[CH:9]=[C:8]([C:7]2[CH:6]=[CH:5][N+:4]([O-:21])=[CH:3][C:2]=2[CH3:1])[CH:20]=[CH:19][CH:18]=1)=[O:12])([CH3:17])([CH3:15])[CH3:16]

참가 물질

5

반응물 2

HCID 784Hydrogen PeroxideHCID 57895121Tert-butyl 3-(3-methylpyridin-4-yl)benzoate

생성물 1

HCID 578951674-(3-(tert-Butoxycarbonyl)phenyl)-3-methylpyridine 1-oxide

시약·촉매·용매 2

HCID 178477782HCID 178477782, 화합물촉매HCID 6344Dichloromethane용매

실험 절차

tert-Butyl 3-(3-methylpyridin-4-yl)benzoate (0.500 g, 1.86 mmol) was dissolved in a mixture of dichloromethane (0.800 mL) and 30% hydrogen peroxide (0.421 mL). Methyltrioxorhenium (VII) (2.3 mg, 0.92 mmol) was added and the reaction mixture was stirred vigorously for 5 hours. The layers were then separated and the organic layer was treated with sodium sulfite, and then dried over sodium sulfate. The crude product filtered, evaporated to dryness, and used without further purification. ESI-MS m/z calc. 285.1. found 286.1 (M+1)+. Retention time 1.22 minutes.

후처리

  1. customThe layers were then separated
  2. additionthe organic layer was treated with sodium sulfite
  3. dry with materialdried over sodium sulfate
  4. filtrationThe crude product filtered
  5. customevaporated to dryness
  6. customused without further purification

출처 및 근거

ORD 기록
ord-fd58781760844103bf1319174b525b1e
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08524910B2

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