Hydrogen Peroxide → 2-(3,5-Dichloro-1-oxido-pyridine-4-yl)-1-{9-methoxy-spiro[2H-1,5-benzodioxepin-3(4H),5'-[1,3]dioxane]-6-yl}ethanone

HRID 2196114

反応式

HRID 2196114 の反応式
[Cl:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Cl:29])[C:7]=1[CH2:8][C:9]([C:11]1[C:26]2[O:25][CH2:24][C:18]3([CH2:23][O:22][CH2:21][O:20][CH2:19]3)[CH2:17][O:16][C:15]=2[C:14]([O:27][CH3:28])=[CH:13][CH:12]=1)=[O:10].[OH:30]O>C(Cl)Cl.C[Re](=O)(=O)=O>[Cl:29][C:6]1[CH:5]=[N+:4]([O-:30])[CH:3]=[C:2]([Cl:1])[C:7]=1[CH2:8][C:9]([C:11]1[C:26]2[O:25][CH2:24][C:18]3([CH2:23][O:22][CH2:21][O:20][CH2:19]3)[CH2:17][O:16][C:15]=2[C:14]([O:27][CH3:28])=[CH:13][CH:12]=1)=[O:10]

参加物

5

反応物 2

HCID 784Hydrogen PeroxideHCID 250055272-(3,5-Dichloropyridin-4-yl)-1-{9-methoxy-spiro[2H-1,5-benzodioxepin-3(4H),5'-[1,3]dioxane]-6-yl}ethanone

生成物 1

HCID 250062622-(3,5-Dichloro-1-oxido-pyridine-4-yl)-1-{9-methoxy-spiro[2H-1,5-benzodioxepin-3(4H),5'-[1,3]dioxane]-6-yl}ethanone

試薬・触媒・溶媒 2

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

実験手順

To a solution of 2-(3,5-Dichloropyridin-4-yl)-1-{9-methoxy-spiro[2H-1,5-benzodioxepin-3(4H),5′-[1,3]dioxane]-6-yl}ethanone [130] (100 mg) in CH2Cl2 (2 mL) was added 30% H2O2 (120 pt) and methyltrioxorhenium(VII) (5 mg). The mixture was stirred for 18 h and subsequently washed with water. The organic phase was dried over MgSO4 and evaporated to dryness under reduced pressure. Standard HPLC purification afforded 85 mg of the product.

後処理

  1. washsubsequently washed with water
  2. dry with materialThe organic phase was dried over MgSO4
  3. customevaporated to dryness under reduced pressure
  4. customStandard HPLC purification

出典と根拠

ORDレコード
ord-fdcee16146a84de0911e2a0e02bb9680
出典データセット
uspto-grants-2012_12
特許番号
US08338431B2

関連ノート

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