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

HRID 2196107

反応式

HRID 2196107 の反応式
[Cl:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Cl:27])[C:7]=1[CH2:8][C:9]([C:11]1[C:24]2[O:23][CH2:22][C:18]3([CH2:21][O:20][CH2:19]3)[CH2:17][O:16][C:15]=2[C:14]([O:25][CH3:26])=[CH:13][CH:12]=1)=[O:10].[OH:28]O>C(Cl)Cl.C[Re](=O)(=O)=O.O=[Mn]=O>[Cl:27][C:6]1[CH:5]=[N+:4]([O-:28])[CH:3]=[C:2]([Cl:1])[C:7]=1[CH2:8][C:9]([C:11]1[C:24]2[O:23][CH2:22][C:18]3([CH2:21][O:20][CH2:19]3)[CH2:17][O:16][C:15]=2[C:14]([O:25][CH3:26])=[CH:13][CH:12]=1)=[O:10]

参加物

6

反応物 2

HCID 784Hydrogen PeroxideHCID 250051682-(3,5-Dichloropyridin-4-yl)-1-{9-methoxy-spiro[2H-1,5-benzodioxepin-3(4H),3'-oxetane]-6-yl}ethanone

生成物 1

HCID 250051692-(3,5-Dichloro-1-oxido-pyridin-4-yl)-1-{9-methoxy-spiro[2H-1,5-benzodioxepin-3(4H),3'-oxetane]-6-yl}ethanone

試薬・触媒・溶媒 3

HCID 14801Manganese dioxide触媒HCID 178477782HCID 178477782、化合物触媒HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 2-(3,5-Dichloropyridin-4-yl)-1-{9-methoxy-spiro[2H-1,5-benzodioxepin-3(4H),3′-oxetane]-6-yl}ethanone [121] (20.5 mg, 50 μmol) in CH2Cl2 (1 mL) was added 30% H2O2 (15 μL) and methyltrioxorhenium(VII) (5 mg). The mixture was stirred for 18 h, added MnO2 (5 mg) and was stirred for another hour. CH2Cl2 (10 mL) was added and the organic phase was washed with water. The combined organic phase was dried over MgSO4 and evaporated to dryness under reduced pressure. Standard HPLC purification afforded 14 mg of the product.

後処理

  1. stirringwas stirred for another hour
  2. washthe organic phase was washed with water
  3. dry with materialThe combined organic phase was dried over MgSO4
  4. customevaporated to dryness under reduced pressure
  5. customStandard HPLC purification

出典と根拠

ORDレコード
ord-0eb6c5e22bcb453e93177ccfb4df0523
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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