Phosphorus oxychloride → 3,4,5-Trichloropyridazine

HRID 568307

反応式

HRID 568307 の反応式
[Cl:1][C:2]1[C:3](=O)[NH:4][N:5]=[CH:6][C:7]=1[Cl:8].P(Cl)(Cl)([Cl:12])=O>>[Cl:12][C:3]1[N:4]=[N:5][CH:6]=[C:7]([Cl:8])[C:2]=1[Cl:1]

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 732474,5-Dichloro-3-hydroxypyridazine

生成物 1

HCID 701113,4,5-Trichloropyridazine

実験手順

A stirred solution of 20.0 grams of 4,5-dichloro-3-pyridazone in 150 ml of phosphorus oxychloride is heated under reflux for five hours. The excess phosphorus oxychloride is removed under reduced pressure, and the residue poured into ice water. The mixture is extracted with diethyl ether. The extract is dried with magnesium sulfate, filtered, and the filtrate concentrated to a residue. The residue is distilled under reduced pressure. A fraction, b.p. 117°-118° C./14-15 mm, 20 grams, solidifies on standing. The solid is recrystallized from acetone-water to yield 3,4,5-trichloropyridazine; m.p. 61° C.

後処理

  1. temperatureunder reflux for five hours
  2. customThe excess phosphorus oxychloride is removed under reduced pressure
  3. additionthe residue poured into ice water
  4. extractionThe mixture is extracted with diethyl ether
  5. dry with materialThe extract is dried with magnesium sulfate
  6. filtrationfiltered
  7. concentrationthe filtrate concentrated to a residue
  8. distillationThe residue is distilled under reduced pressure
  9. customThe solid is recrystallized from acetone-water

出典と根拠

ORDレコード
ord-1b32c944f3204d678de1d668cb4a71fb
出典データセット
uspto-grants-1988_03
特許番号
US04728355

関連ノート

読み込み中…