Phosphorus pentachloride → HCID 68677101, compound

HRID 1985873Notes

Reaction equation

HRID 1985873 reaction equation
[C:1]([N:4]1[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([Cl:13])[CH:11]=2)[C:6](=[C:14](O)[C:15]2[CH:20]=[CH:19][C:18]([C:21]#[N:22])=[CH:17][CH:16]=2)[C:5]1=[O:24])(=[O:3])[CH3:2].P(Cl)(Cl)(Cl)(Cl)[Cl:26]>O1CCOCC1>[C:1]([N:4]1[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([Cl:13])[CH:11]=2)[C:6](=[C:14]([Cl:26])[C:15]2[CH:20]=[CH:19][C:18]([C:21]#[N:22])=[CH:17][CH:16]=2)[C:5]1=[O:24])(=[O:3])[CH3:2]

Participants

4

Reactant 2

HCID 24819Phosphorus pentachloride2×HCID 178473969HCID 178473969, compound

Product 1

HCID 68677101HCID 68677101, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Conditions

Temperature
100 °C

Procedure

A suspension of 7.0 g of 1-acetyl-3-[1-hydroxy-1-(4-cyanophenyl)methylene]-6-chloro-2-indolinone (starting material VI.18) and 6.39 g of phosphorus pentachloride in 150 ml of dioxane is stirred at 100° C. for 6 hours. After addition of a further 1.0 g of phosphorus pentachloride, the mixture is stirred at 110° C. for another 4 hours. The solvent is then distilled off and the residue is washed with ethyl acetate.

Workup

  1. stirringthe mixture is stirred at 110° C. for another 4 hours
  2. distillationThe solvent is then distilled off
  3. washthe residue is washed with ethyl acetate

Sources & evidence

ORD record
ord-1dd5ae70392b445597fa7d897599bfff
Source dataset
uspto-grants-2009_06
Patent number
US07547703B2

Reaction notes

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