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

반응식

HRID 2196107 반응식
[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]

참가 물질

6

반응물 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

생성물 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

시약·촉매·용매 3

HCID 14801Manganese dioxide촉매HCID 178477782HCID 178477782, 화합물촉매HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0eb6c5e22bcb453e93177ccfb4df0523
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08338431B2

연결된 노트

불러오는 중…