Carbon Tetrachloride → HCID 21188095, compound

HRID 1383588Notes

Reaction equation

HRID 1383588 reaction equation
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[C:20]([Cl:24])(Cl)(Cl)[Cl:21].[C:25]([C:27]1[C:31]([CH:32]=O)=[CH:30][N:29]([C:34]2[C:39]([Cl:40])=[CH:38][C:37]([C:41]([F:44])([F:43])[F:42])=[CH:36][C:35]=2[Cl:45])[N:28]=1)#[N:26]>ClCCl>[C:25]([C:27]1[C:31]([CH:32]=[C:20]([Cl:24])[Cl:21])=[CH:30][N:29]([C:34]2[C:39]([Cl:40])=[CH:38][C:37]([C:41]([F:42])([F:44])[F:43])=[CH:36][C:35]=2[Cl:45])[N:28]=1)#[N:26]

Participants

5

Reactant 3

HCID 5943Carbon TetrachlorideHCID 11776TriphenylphosphineHCID 184179813-Cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)4-formylpyrazole

Product 1

HCID 21188095HCID 21188095, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

A solution of triphenylphosphine (0.983 g) and carbon tetrachloride (0.145 ml) in anhydrous dichloromethane (5 ml) at 0° C. was stirred for 5 minutes. 3-Cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-formylpyrazole (0.25 g) was then added and the mixture was heated under reflux for 5 hours and then evaporated. The residue was purified by column chromatography on silica gel eluting with dichloromethane. Combination and evaporation of suitable fractions gave the title compound as a white solid, m.p. 99-101° C.

Workup

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 5 hours
  3. customevaporated
  4. customThe residue was purified by column chromatography on silica gel eluting with dichloromethane
  5. customCombination and evaporation of suitable fractions

Sources & evidence

ORD record
ord-1ad8ba7284af4e34a27a1f0ee154b336
Source dataset
uspto-grants-2001_07
Patent number
US06255333B1

Reaction notes

Loading…