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

HRID 1154148

반응식

HRID 1154148 반응식
[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]

참가 물질

4

반응물 2

HCID 24638Chlorosulfonic acidHCID 885552,3,5-Trimethylanisole

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d3ead4adc2794510a0bb27b474514578
출처 데이터셋
uspto-grants-1984_12
특허 번호
US04487726

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