Chlorosulfonic acid → HCID 15220190, compound

HRID 583045Notes

Reaction equation

HRID 583045 reaction equation
[Cl:1][C:2]1[C:3]([C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][CH:13]=2)=[N:4][N:5]([CH3:11])[C:6]=1[O:7][CH:8]([F:10])[F:9].[Cl:19][S:20](O)(=[O:22])=[O:21]>>[Cl:1][C:2]1[C:3]([C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[C:14]([S:20]([Cl:19])(=[O:22])=[O:21])[CH:13]=2)=[N:4][N:5]([CH3:11])[C:6]=1[O:7][CH:8]([F:9])[F:10]

Participants

3

Reactant 2

HCID 24638Chlorosulfonic acidHCID 15220185HCID 15220185, compound

Product 1

HCID 15220190HCID 15220190, compound

Conditions

Temperature
130 °C

Procedure

47.9 g (0.16 mol) of 4-chloro-3-(4-chlorophenyl)-5-difluoromethoxy-1-methyl-1H-pyrazole were added a little at a time at 0° C. to 91 ml of chlorosulfonic acid. The mixture was stirred at 130° C. for 4 hours and then cooled, and the solution was poured carefully into ice-water. Product dissolved in the aqueous phase was extracted twice with dichloromethane. The combined organic phases were subsequently washed with saturated sodium hydrogen carbonate solution and with sodium chloride solution, then dried over magnesium sulfate and finally concentrated. Yield: 47.9 g.

Workup

  1. temperaturecooled
  2. dissolutionProduct dissolved in the aqueous phase
  3. extractionwas extracted twice with dichloromethane
  4. washThe combined organic phases were subsequently washed with saturated sodium hydrogen carbonate solution and with sodium chloride solution
  5. dry with materialdried over magnesium sulfate
  6. concentrationfinally concentrated

Sources & evidence

ORD record
ord-3150176bc5f74a0fabfe4203ca242cb8
Source dataset
uspto-grants-1999_07
Patent number
US05928999

Reaction notes

Loading…