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

HRID 1154146

반응식

HRID 1154146 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c254c37c89bf40f29c916ef78cc2ef2d
출처 데이터셋
uspto-grants-1984_12
특허 번호
US04487726

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