Phosphorus pentachloride → HCID 13172332、化合物

HRID 1863491ノート

反応式

HRID 1863491 の反応式
[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]

参加物

3

反応物 2

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

生成物 1

HCID 13172332HCID 13172332、化合物

実験手順

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 ninety 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°.

後処理

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

出典と根拠

ORDレコード
ord-52ebf5a208fc41fc9422f8573d45242f
出典データセット
uspto-grants-1979_09
特許番号
US04169153

反応ノート

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