Phosphorus oxychloride → HCID 22618466, compound

HRID 1078436Notes

Reaction equation

HRID 1078436 reaction equation
P(Cl)(Cl)(Cl)=O.[NH2:6][C:7]1[N:11]([C:12]2[C:17]([Cl:18])=[CH:16][C:15]([C:19]([F:22])([F:21])[F:20])=[CH:14][C:13]=2[Br:23])[N:10]=[C:9]([C:24](=O)[NH2:25])[C:8]=1[S:27]([CH3:30])(=[O:29])=[O:28]>O>[NH2:6][C:7]1[N:11]([C:12]2[C:17]([Cl:18])=[CH:16][C:15]([C:19]([F:21])([F:22])[F:20])=[CH:14][C:13]=2[Br:23])[N:10]=[C:9]([C:24]#[N:25])[C:8]=1[S:27]([CH3:30])(=[O:29])=[O:28]

Participants

4

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 22618482HCID 22618482, compound

Product 1

HCID 22618466HCID 22618466, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

Phosphorus oxychloride (20 ml) was added to 5-amino-1-(2-bromo-6-chloro-4-trifluoromethylphenyl)-3-carbamoyl-4-methanesulphonylpyrazole (4.0 g) and the solution heated at 50°-60° C. for 3.25 hours, and left at room temperature overnight. The mixture was cautiously added to vigorously stirred water (200 ml), and the precipitated solid collected and dried in vacuo. Recrystallisation from toluene/ethanol gave 5-amino-1-(2-bromo-6-chloro-4-trifluoromethylphenyl)-3-cyano-4-methanesulphonylpyrazole as buff crystals, m.p. 235°-238° C.

Workup

  1. temperaturethe solution heated at 50°-60° C. for 3.25 hours
  2. customthe precipitated solid collected
  3. customdried in vacuo
  4. customRecrystallisation from toluene/ethanol

Sources & evidence

ORD record
ord-2ef13ad80664425a9edb2b1151925c55
Source dataset
uspto-grants-1996_08
Patent number
US05547974

Reaction notes

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