Chlorosulfonic acid → 8-Methoxy-7-chlorosulfonyl-1,4-benzodioxane-5-carboxylic acid

HRID 1660017Notes

Reaction equation

HRID 1660017 reaction equation
[CH3:1][O:2][C:3]1[C:8]2[O:9][CH2:10][CH2:11][O:12][C:7]=2[C:6]([C:13]([OH:15])=[O:14])=[CH:5][CH:4]=1.[Cl:16][S:17](O)(=[O:19])=[O:18]>>[CH3:1][O:2][C:3]1[C:8]2[O:9][CH2:10][CH2:11][O:12][C:7]=2[C:6]([C:13]([OH:15])=[O:14])=[CH:5][C:4]=1[S:17]([Cl:16])(=[O:19])=[O:18]

Participants

3

Reactant 2

HCID 24638Chlorosulfonic acidHCID 227342488-Methoxy-2,3-dihydrobenzo[b][1,4]dioxine-5-carboxylic Acid

Product 1

HCID 205447488-Methoxy-7-chlorosulfonyl-1,4-benzodioxane-5-carboxylic acidYield 98%

Procedure

1045 cm3 of chlorosulfonic acid were introduced into a balloon flask provided with an agitator, a thermometer and a condenser and then, in portions, 110 g of 8-methoxy-1,4-benzodioxane-5-carboxylic acid were added with the temperature being maintained at from 5°-10° C. The mixture was agitated at ambient temperature and then poured on ice. The precipitate was dried off, washed and dried. 159 g of 8-methoxy-7-chlorosulfonyl-1,4-benzodioxane-5-carboxylic acid were obtained (yield: 98%).

Workup

  1. customprovided with an agitator
  2. temperaturebeing maintained at from 5°-10° C
  3. additionpoured on ice
  4. customThe precipitate was dried off
  5. washwashed
  6. customdried

Sources & evidence

ORD record
ord-c3f3ee60cd844bfba15e4013bdd2eb2d
Source dataset
uspto-grants-1981_12
Patent number
US04306072

Reaction notes

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