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

반응식

HRID 2196114 반응식
[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]

참가 물질

5

반응물 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

생성물 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

시약·촉매·용매 2

HCID 178477782HCID 178477782, 화합물촉매HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fdcee16146a84de0911e2a0e02bb9680
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08338431B2

연결된 노트

불러오는 중…