Phosphorus oxychloride → HCID 22618466, compound

HRID 1416814Notes

Reaction equation

HRID 1416814 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. 225-238 ° C.

Workup

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

Sources & evidence

ORD record
ord-b6483a5f6ca94b76b2020cc6686ec184
Source dataset
uspto-grants-1999_06
Patent number
US05916618

Reaction notes

Loading…