Phosphorus pentachloride → HCID 13172332、化合物

HRID 372361ノート

反応式

HRID 372361 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 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°.

後処理

  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

出典と根拠

ORDレコード
ord-2b2a1d6b3f7f44aa8710dea916f3f4b5
出典データセット
uspto-grants-1978_05
特許番号
US04091011

反応ノート

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