Sulfuryl chloride → HCID 15220185, compound
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
Product 1
Reagents, catalysts & solvents 1
Procedure
A solution of 74.0 g (0,549 mol) of sulfuryl chloride in 200 ml of carbon tetrachloride was added slowly 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. After the exothermic reaction with evolution of gas had subsided, the reaction mixture was stirred at 20°-25° C.for 2 hours more. The reaction solution was then washed with water, saturated sodium hydrogen carbonate solution and saturated sodium chloridesolution, and finally 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
- customAfter the exothermic reaction with evolution of gas
- washThe reaction solution was then washed with water, saturated sodium hydrogen carbonate solution and saturated sodium chloridesolution
- customfinally dried
- concentrationconcentrated
Sources & evidence
- ORD record
- ord-e4813aab34134dc1920ec1beeee0164b
- Source dataset
- uspto-grants-1998_04
- Patent number
- US05744426
Reaction notes
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