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

HRID 1167247
ノート
印刷プレビュー

反応式

HRID 1167247 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 24638Chlorosulfonic acidHCID 295722,5-Dichlorotoluene

生成物 1

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

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4aa8bc8e7f39416b9f73f8c00afc4573
出典データセット
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06617357B2

反応ノート

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