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m-Chloroperbenzoic acid → 5-Bromo-2-[(2,6-dichlorophenyl)methanesulfinyl]-1-oxo-1lambda~5~-pyridine

HRID 1980213
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HRID 1980213 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([S:9][CH2:10][C:11]2[C:16]([Cl:17])=[CH:15][CH:14]=[CH:13][C:12]=2[Cl:18])=[N+:6]([O-:8])[CH:7]=1.ClC1C=CC=C(C(OO)=[O:27])C=1>C(Cl)(Cl)Cl>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([S:9]([CH2:10][C:11]2[C:12]([Cl:18])=[CH:13][CH:14]=[CH:15][C:16]=2[Cl:17])=[O:27])=[N+:6]([O-:8])[CH:7]=1
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참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 204023455-Bromo-2-{[(2,6-dichlorophenyl)methyl]sulfanyl}-1-oxo-1lambda~5~-pyridine

생성물 1

HCID 134778795-Bromo-2-[(2,6-dichlorophenyl)methanesulfinyl]-1-oxo-1lambda~5~-pyridine수율 83.3%

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

2.3 g of 5-bromo-2-(2,6-dichlorobenzylthio)pyridine-N-oxide was dissolved in 50 ml of chloroform, and a solution of 1.6 g of metachloroperbenzoic acid (content: 70%) dissolved in 30 ml of chloroform was added dropwise thereto at 5° to 10° C. over 10 minutes. The mixture was stirred at 5° to 10° C. for an additional 2 hours. The resulting mixture was washed twice with potassium carbonate solution and dried over magnesium sulfate. The chloroform was evaporated, and the residue was recrystallized from benzene to obtain 2.0 g of 5-bromo-2-(2,6-dichlorobenzylsulfinyl)pyridine-N-oxide (Compound (2)). Yield, 83%. M.P., 187.5°-188.5° C.

후처리

  1. additionwas added dropwise
  2. washThe resulting mixture was washed twice with potassium carbonate solution
  3. dry with materialdried over magnesium sulfate
  4. customThe chloroform was evaporated
  5. customthe residue was recrystallized from benzene

출처 및 근거

ORD 기록
ord-3efb462294d0495582ae0fc3b71e2629
출처 데이터셋
uspto-grants-1985_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04508562

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