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2,6-Dichlorotoluene → 2,4-Dichloro-3-methylbenzene-1-sulfonyl chloride

HRID 1990717
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HRID 1990717 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[CH3:9].[Cl:10][S:11](O)(=[O:13])=[O:12]>>[Cl:1][C:2]1[C:3]([CH3:9])=[C:4]([Cl:8])[CH:5]=[CH:6][C:7]=1[S:11]([Cl:10])(=[O:13])=[O:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 83682,6-DichlorotolueneHCID 24638Chlorosulfonic acid

생성물 1

HCID 157253742,4-Dichloro-3-methylbenzene-1-sulfonyl chloride수율 85%

실험 절차

10 ml of chlorosulfonic acid were dropwise added with 4.8 ml of 2,6-dichlorotoluene in two hours, under magnetic stirring at room temperature. After completion of the addition, the mixture was heated at 40° C. for two hours, thereby obtaining a purple solution, which was cooled and carefully poured into ice-water (0.5 l), stirring vigorously. The separated white solid was filtered, triturated, washed with water, dried over KOH and purified by washing with n-hexane, adding 200 ml of solvent under strong stirring. The mixture was filtered, the solid was discarded and the solvent was evaporated to dryness to obtain 2,4-dichloro-3-methyl-benzenesulfonyl chloride as a crystalline white solid. Yield: 85%.

후처리

  1. additionAfter completion of the addition
temperature
the mixture was heated at 40° C. for two hours
  • customobtaining a purple solution, which
  • temperaturewas cooled
  • stirringstirring vigorously
  • filtrationThe separated white solid was filtered
  • customtriturated
  • washwashed with water
  • dry with materialdried over KOH
  • custompurified
  • washby washing with n-hexane
  • additionadding 200 ml of solvent under strong stirring
  • filtrationThe mixture was filtered
  • customthe solvent was evaporated to dryness
  • 출처 및 근거

    ORD 기록
    ord-914016fb3d204dc2b3f71db600191261
    출처 데이터셋
    uspto-grants-2010_01
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US07645759B2

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