Carbon Tetrachloride → HCID 19096768, compound

HRID 486876Notes

Reaction equation

HRID 486876 reaction equation
[Cl:1][C:2]1[C:7]([O:8][CH2:9][C:10]#[CH:11])=[CH:6][C:5]([NH:12][C:13](=O)[CH2:14][Cl:15])=[C:4]([F:17])[CH:3]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Cl)(Cl)(Cl)[Cl:38]>ClCCCl>[Cl:1][C:2]1[C:7]([O:8][CH2:9][C:10]#[CH:11])=[CH:6][C:5]([N:12]=[C:13]([Cl:38])[CH2:14][Cl:15])=[C:4]([F:17])[CH:3]=1

Participants

5

Reactant 3

HCID 5943Carbon TetrachlorideHCID 11776TriphenylphosphineHCID 19096763HCID 19096763, compound

Product 1

HCID 19096768HCID 19096768, compound

Reagents, catalysts & solvents 1

HCID 111,2-DichloroethaneSolvent

Procedure

First, 2.00 g of N-(4-chloro-2-fluoro-5-propargyloxyphenyl)-2-chloroacetamide, 4.50 g of triphenylphosphine and 5 ml of carbon tetrachloride were dissolved in 45 ml of 1,2-dichloroethane, and then the reflux under heat was continued for 2 hr. After letting the solution stand to cool the same, the solvent was distilled out under reduced pressure, and then the residue was refined by silica gel column chromatography (effluent: ethyl acetate/n-hexane (v/v)=6/4) to obtain 1.43 g of N-(4-chloro-2-fluoro-5-propargyloxyphenyl)-2-chloroacetimidoylchloride. The boiling point was 144°-146° C./0.4 mm Hg.

Workup

  1. temperaturethe reflux
  2. temperatureunder heat
  3. temperatureto cool the same, the solvent
  4. distillationwas distilled out under reduced pressure

Sources & evidence

ORD record
ord-a0db4b91eca74f0a985c938d72e6f25f
Source dataset
uspto-grants-1994_03
Patent number
US05292922

Reaction notes

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