Chlorosulfonic acid → 4-Methoxy-2,3,6-trimethylbenzenesulfonyl chloride

HRID 1154148

反応式

HRID 1154148 の反応式
[CH3:1][C:2]1[C:7]([CH3:8])=[CH:6][C:5]([CH3:9])=[CH:4][C:3]=1[O:10][CH3:11].[Cl:12][S:13](O)(=[O:15])=[O:14]>C(Cl)Cl>[CH3:11][O:10][C:3]1[CH:4]=[C:5]([CH3:9])[C:6]([S:13]([Cl:12])(=[O:15])=[O:14])=[C:7]([CH3:8])[C:2]=1[CH3:1]

参加物

4

反応物 2

HCID 24638Chlorosulfonic acidHCID 885552,3,5-Trimethylanisole

生成物 1

HCID 5627874-Methoxy-2,3,6-trimethylbenzenesulfonyl chloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

In 500 ml of methylenchloride was dissolved 4.5 g of 2,3,5-trimethylanisole, and after cooling at -5°~-10° C., a solution (400 ml) of 6.0 ml of chlorosulfonic acid in methylene chloride was added dropwise to the mixture. The reaction mixture was kept at room temperature and then poured into ice-5% aqueous NaHCO3. The methylene chloride layer was washed with water and dried over anhydrous magnesium sulfate. The solvent was distilled off and the residue was crystallized from n-hexane and filtered.

後処理

  1. temperatureafter cooling at -5°~-10° C.
  2. customwas kept at room temperature
  3. washThe methylene chloride layer was washed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationThe solvent was distilled off
  6. customthe residue was crystallized from n-hexane
  7. filtrationfiltered

出典と根拠

ORDレコード
ord-d3ead4adc2794510a0bb27b474514578
出典データセット
uspto-grants-1984_12
特許番号
US04487726

関連ノート

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