Phosphorus oxide (P4O10) → HCID 22618419, compound

HRID 2253769Notes

Reaction equation

HRID 2253769 reaction equation
[C:1]([C:4]1[N:8]([C:9]2[C:14]([Cl:15])=[CH:13][C:12]([C:16]([F:19])([F:18])[F:17])=[CH:11][C:10]=2[Cl:20])[N:7]=[C:6]([C:21]([F:24])([F:23])[F:22])[C:5]=1[C:25]#[N:26])(=O)[NH2:2].O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>>[Cl:20][C:10]1[CH:11]=[C:12]([C:16]([F:17])([F:19])[F:18])[CH:13]=[C:14]([Cl:15])[C:9]=1[N:8]1[C:4]([C:1]#[N:2])=[C:5]([C:25]#[N:26])[C:6]([C:21]([F:23])([F:24])[F:22])=[N:7]1

Participants

3

Reactant 2

HCID 14812Phosphorus oxide (P4O10)HCID 10223681HCID 10223681, compound

Product 1

HCID 22618419HCID 22618419, compound

Procedure

5-Carbamoyl-4-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-trifluoromethylpyrazole (3.57 g) was heated to 200° C. with phosphorus pentoxide (2.82 g) with stirring. After 3 hours, the cooled product was treated with ice, and extracted with dichloromethane (3×50 ml). The organic solution was washed with water, dried over anhydrous magnesium sulphate, and evaporated in vacuo to give a solid. Recrystallization from hexane gave 1-(2,6-dichloro-4-trifluoromethylphenyl)-4,5-dicyano-3-trifluoromethylpyrazole in the form of white crystals (1.8 g), m.p. 80° C.

Workup

  1. additionthe cooled product was treated with ice
  2. extractionextracted with dichloromethane (3×50 ml)
  3. washThe organic solution was washed with water
  4. dry with materialdried over anhydrous magnesium sulphate
  5. customevaporated in vacuo
  6. customto give a solid
  7. customRecrystallization from hexane

Sources & evidence

ORD record
ord-3f8d581cd2e1472ba7f90046280aa13f
Source dataset
uspto-grants-1993_08
Patent number
US05232940

Reaction notes

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