Phosphorus oxychloride → HCID 22618466, compound

HRID 842140Notes

Reaction equation

HRID 842140 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

Conditions

Temperature
55 °C

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. customthe precipitated solid collected
  2. customdried in vacuo
  3. customRecrystallisation from toluene/ethanol

Sources & evidence

ORD record
ord-4e8252ec590c4675b9374ba45c25214a
Source dataset
uspto-grants-2002_04
Patent number
US06372774B1

Reaction notes

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