HCID 18781569, compound → HCID 18781570, compound

HRID 1421395Notes

Reaction equation

HRID 1421395 reaction equation
[C:1]1([P:7]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([C:15]([F:18])([F:17])[F:16])[C:10]=2I)=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1>CN(C)C=O.[Cu]>[C:1]1([P:7]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([C:15]([F:18])([F:17])[F:16])[C:10]=2[C:10]2[C:11]([C:15]([F:17])([F:18])[F:16])=[CH:12][CH:13]=[CH:14][C:9]=2[P:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[O:8])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Participants

4

Reactant 1

HCID 18781569HCID 18781569, compound

Product 1

HCID 18781570HCID 18781570, compound

Reagents, catalysts & solvents 2

HCID 23978CopperCatalystHCID 6228DimethylformamideSolvent

Conditions

Temperature
100 °C

Procedure

In a nitrogen atmosphere, 4.16 g (8.81 mmol) of 1-(diphenylphosphinyl)-2-iodo-3-trifluoromethyl benzene was dissolved in 40 ml of dimethyl formamide, and 1.5 g of copper powder was added and stirred for 30 minutes at 100° C. After allowing to cool, dimethyl formamide was distilled away in vacuo, and the residue was refined by chromatography (SiO2 70 g, CHCl3). By recrystallizing with ethyl acetate, 0.64 g (21%) of the captioned compound in the form of a white crystal was obtained.

Workup

  1. temperatureto cool
  2. distillationdimethyl formamide was distilled away in vacuo
  3. customBy recrystallizing with ethyl acetate, 0.64 g (21%) of the captioned compound in the form of a white crystal
  4. customwas obtained

Sources & evidence

ORD record
ord-31bd788da26640dda022e6b94ed37e48
Source dataset
uspto-grants-2000_06
Patent number
US06075154

Reaction notes

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