Sulfuryl chloride → HCID 15220185, compound

HRID 583035Notes

Reaction equation

HRID 583035 reaction equation
S(Cl)([Cl:4])(=O)=O.[Cl:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[CH:17]=[C:16]([O:18][CH:19]([F:21])[F:20])[N:15]([CH3:22])[N:14]=2)=[CH:9][CH:8]=1>C(Cl)(Cl)(Cl)Cl>[Cl:4][C:17]1[C:13]([C:10]2[CH:9]=[CH:8][C:7]([Cl:6])=[CH:12][CH:11]=2)=[N:14][N:15]([CH3:22])[C:16]=1[O:18][CH:19]([F:21])[F:20]

Participants

4

Reactant 2

HCID 24648Sulfuryl chlorideHCID 15220184HCID 15220184, compound

Product 1

HCID 15220185HCID 15220185, compound

Reagents, catalysts & solvents 1

HCID 5943Carbon TetrachlorideSolvent2×

Conditions

Temperature
20 °C

Procedure

74.0 g (0.549 mol) of sulfuryl chloride dissolved in 200 ml of carbon tetrachloride were added slowly dropwise to a solution of 128.9 g (0.5 mol) of 3-(4-chlorophenyl)-5-difluoromethoxy-1-methyl-1H-pyrazole in 500 ml of carbon tetrachloride, the ensuing reaction being exothermic with evolution of gas. After the end of the reaction the mixture was stirred at about 20° C. for a further 2 h. The reaction solution was then washed with about 300 ml each of water, saturated sodium hydrogen carbonate solution and saturated sodium chloride solution, and then dried and concentrated. Yield: 139.3 g; 1H-NMR (270 MHz, in CDCl3): δ [ppm]=7.79 (d, 2H), 7.43 (d, 2H), 6.70 (t, 1H), 3.85 (s, 3H).

Workup

  1. customthe ensuing reaction
  2. customAfter the end of the reaction the mixture
  3. washThe reaction solution was then washed with about 300 ml each of water, saturated sodium hydrogen carbonate solution and saturated sodium chloride solution
  4. customdried
  5. concentrationconcentrated

Sources & evidence

ORD record
ord-b3c2810234734df6ac217d2d737b6766
Source dataset
uspto-grants-1999_07
Patent number
US05928999

Reaction notes

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