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

HRID 39453

反応式

HRID 39453 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 178477782HCID 178477782、化合物触媒HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-fd58781760844103bf1319174b525b1e
出典データセット
uspto-grants-2013_09
特許番号
US08524910B2

関連ノート

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