Phosphorus oxychloride → 3,4,5-Trichloropyridazine

HRID 568307

반응식

HRID 568307 반응식
[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]

참가 물질

3

반응물 2

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

생성물 1

HCID 701113,4,5-Trichloropyridazine

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1b32c944f3204d678de1d668cb4a71fb
출처 데이터셋
uspto-grants-1988_03
특허 번호
US04728355

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