Chlorosulfonic acid → 52499-93-1

HRID 1856254Notes

Reaction equation

HRID 1856254 reaction equation
[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]

Participants

3

Reactant 2

HCID 24638Chlorosulfonic acidHCID 693011,3,5-Trimethoxybenzene

Product 1

HCID 1591751952499-93-1

Procedure

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.

Workup

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

Sources & evidence

ORD record
ord-c91a3f6584184aaa8fcfc9c0aff9073b
Source dataset
uspto-grants-1980_08
Patent number
US04218476

Reaction notes

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