Chlorosulfonic acid → 845616-29-7

HRID 1930990Notes

Reaction equation

HRID 1930990 reaction equation
[F:1][C:2]([F:14])([F:13])[O:3][C:4]1[CH:12]=[CH:11][CH:10]=[CH:9][C:5]=1[C:6]([OH:8])=[O:7].[Cl:15][S:16](O)(=[O:18])=[O:17]>>[Cl:15][S:16]([C:10]1[CH:11]=[CH:12][C:4]([O:3][C:2]([F:13])([F:14])[F:1])=[C:5]([CH:9]=1)[C:6]([OH:8])=[O:7])(=[O:18])=[O:17]

Participants

3

Reactant 2

HCID 24638Chlorosulfonic acidHCID 27772232-(Trifluoromethoxy)benzoic acid

Product 1

HCID 86600705845616-29-7

Conditions

Temperature
70 °C

Procedure

A solution of 2-trifluoromethoxy benzoic acid [1979-29-9] (1.0 g) was added in small batches to chlorosulfonic acid (3.2 mL) at 0° C. After completion of the addition, the reaction mixture was stirred at 70° C. for 4 hours then left at room temperature overnight and heated at 75° C. for another 3 hours. After such time the reaction was slowly poured onto ice, and the precipitate was then filtered, washed with water and dried to yield the title compound as a white solid (1.2 g). MS (m/e): 303.3 (M−H, 100%).

Workup

  1. additionAfter completion of the addition
  2. waitthen left at room temperature overnight
  3. temperatureheated at 75° C. for another 3 hours
  4. additionAfter such time the reaction was slowly poured onto ice
  5. filtrationthe precipitate was then filtered
  6. washwashed with water
  7. customdried

Sources & evidence

ORD record
ord-710f453a539e45bdb94a4d0cf855b718
Source dataset
uspto-grants-2012_05
Patent number
US08188139B2

Reaction notes

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