Phosphorus pentachloride → HCID 13172332, compound

HRID 372361Notes

Reaction equation

HRID 372361 reaction equation
[Cl:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[C:9]([Cl:14])[C:8]([N+:15]([O-:17])=[O:16])=[CH:7][C:3]=1[C:4](O)=[O:5].P(Cl)(Cl)(Cl)(Cl)[Cl:19]>>[Cl:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[C:9]([Cl:14])[C:8]([N+:15]([O-:17])=[O:16])=[CH:7][C:3]=1[C:4]([Cl:19])=[O:5]

Participants

3

Reactant 2

HCID 24819Phosphorus pentachlorideHCID 964972,4-Dichloro-3,5-dinitrobenzoic acid

Product 1

HCID 13172332HCID 13172332, compound

Procedure

A mixture of 75.0 g. (0.2669 mole) of 2,4-dichloro-3,5-dinitrobenzoic acid and 55.59 g. (0.2669 mole) of phosphorus pentachloride is heated at reflux for 90 minutes and cooled to room temperature. The phosphorus oxychloride is distilled off in vacuo. The residue is recrystallized from cyclohexane to yield 75.9 gm. (95%) of yellow needles melting at 99°-101°.

Workup

  1. additionA mixture of 75.0 g
  2. temperatureat reflux for 90 minutes
  3. distillationThe phosphorus oxychloride is distilled off in vacuo
  4. customThe residue is recrystallized from cyclohexane
  5. customto yield 75.9 gm

Sources & evidence

ORD record
ord-2b2a1d6b3f7f44aa8710dea916f3f4b5
Source dataset
uspto-grants-1978_05
Patent number
US04091011

Reaction notes

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