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Chlorosulfonic acid → 2,5-Dichloro-4-methylbenzene-1-sulfonyl chloride

HRID 1167247
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HRID 1167247 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1[CH3:9].[Cl:10][S:11](O)(=[O:13])=[O:12]>>[Cl:8][C:5]1[CH:4]=[C:3]([CH3:9])[C:2]([Cl:1])=[CH:7][C:6]=1[S:11]([Cl:10])(=[O:13])=[O:12]
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참가 물질

3

반응물 2

HCID 24638Chlorosulfonic acidHCID 295722,5-Dichlorotoluene

생성물 1

HCID 134912212,5-Dichloro-4-methylbenzene-1-sulfonyl chloride수율 88%

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온도
0 °C

실험 절차

A dry flask under argon was charged with chlorosulfonic acid (30 mL) and cooled to 0° C. 2,5-Dichlorotoluene (10 g, 62.1 mmol) was then added dropwise, and once the addition was complete, the reaction was heated to 60° C. and stirred for 30 min. After cooling to room temperature, the reaction mixture was poured slowly onto ice. The aqueous mixture was extracted twice with methylene chloride, and the organics were dried and concentrated to provide 2,5-dichloro-4-methylbenzenesulfonyl chloride (14.14 g, 88%) as a white solid.

후처리

  1. additiononce the addition
  2. temperaturethe reaction was heated to 60° C.
  3. temperatureAfter cooling to room temperature
  4. additionthe reaction mixture was poured slowly onto ice
  5. extractionThe aqueous mixture was extracted twice with methylene chloride
  6. customthe organics were dried
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-4aa8bc8e7f39416b9f73f8c00afc4573
출처 데이터셋
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06617357B2

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