Chlorosulfonic acid → 4-Methoxy-2,3,5,6-tetramethylbenzenesulfonyl chloride

HRID 1164286

反応式

HRID 1164286 の反応式
[CH3:1][C:2]1[C:7]([CH3:8])=[CH:6][C:5]([CH3:9])=[C:4]([CH3:10])[C:3]=1[O:11][CH3:12].[Cl:13][S:14](O)(=[O:16])=[O:15]>ClCCl>[CH3:12][O:11][C:3]1[C:4]([CH3:10])=[C:5]([CH3:9])[C:6]([S:14]([Cl:13])(=[O:16])=[O:15])=[C:7]([CH3:8])[C:2]=1[CH3:1]

参加物

4

反応物 2

HCID 24638Chlorosulfonic acidHCID 2786643-Methoxy-1,2,4,5-tetramethylbenzene

生成物 1

HCID 159175204-Methoxy-2,3,5,6-tetramethylbenzenesulfonyl chloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

In 600 ml of dichloromethane was dissolved 10.0 g of 2,3,5,6-tetramethylanisole, followed by addition of a solution (400 ml) of 12 ml of chlorosulfonic acid in dichloromethane at -5°~-10° C. The mixture was kept stirred for 2 hours and the reaction mixture was poured into ice-5% aqueous NaHCO3. The organic layer was washed with water and dried over magnesium sulfate. The solvent was distilled off and the residue was crystallized from n-hexane and filtered.

後処理

  1. washThe organic layer was washed with water
  2. dry with materialdried over magnesium sulfate
  3. distillationThe solvent was distilled off
  4. customthe residue was crystallized from n-hexane
  5. filtrationfiltered

出典と根拠

ORDレコード
ord-87c3f7ec7fab4194a04023d4475c0f29
出典データセット
uspto-grants-1983_01
特許番号
US04368150

関連ノート

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