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

HRID 1856254
ノート
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反応式

HRID 1856254 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 24638Chlorosulfonic acidHCID 693011,3,5-Trimethoxybenzene

生成物 1

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

実験手順

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.

後処理

  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
  • 出典と根拠

    ORDレコード
    ord-c91a3f6584184aaa8fcfc9c0aff9073b
    出典データセット
    uspto-grants-1980_08
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US04218476

    反応ノート

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