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Chlorosulfonic acid → 2,4,6-Trimethoxybenzene-1-sulfonyl chloride

HRID 1856254
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HRID 1856254 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[CH:6]=[C:5]([O:11][CH3:12])[CH:4]=1.[Cl:13][S:14](O)(=[O:16])=[O:15]>>[CH3:12][O:11][C:5]1[CH:4]=[C:3]([O:2][CH3:1])[CH:8]=[C:7]([O:9][CH3:10])[C:6]=1[S:14]([Cl:13])(=[O:16])=[O:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 24638Chlorosulfonic acidHCID 693011,3,5-Trimethoxybenzene

생성물 1

HCID 159175192,4,6-Trimethoxybenzene-1-sulfonyl chloride

실험 절차

16.8 g (0.1 mole) 1,3,5 -trimethoxybenzene were added in portions to 33 ml chlorosulphonic acid, giving a clear pale-yellow solution. The solution was allowed to stand at about 20° C. for 2 hours and was then poured onto ice. The crystals formed were collected, washed with water, taken up in CHCl3, washed with water, and dried with sodium sulphate. The solvent was removed in vacuum, giving 15 g of the crude title compound. The crude product was dissolved in a minimum of hot CHCl3 and di-isopropylether was added. After cooling, white crystals of title compound (9 g) were collected; m.p. 134°-136° C.

후처리

  1. customgiving a clear pale-yellow solution
  2. additionwas then poured onto ice
  3. customThe crystals formed
  4. customwere collected
  • washwashed with water
  • washwashed with water
  • dry with materialdried with sodium sulphate
  • customThe solvent was removed in vacuum
  • 출처 및 근거

    ORD 기록
    ord-c91a3f6584184aaa8fcfc9c0aff9073b
    출처 데이터셋
    uspto-grants-1980_08
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04218476

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