Phosphorus oxychloride → 3-(3-Bromo-4-methoxyphenyl)-6-chloropyridazine

HRID 1763578ノート

反応式

HRID 1763578 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([C:10]2[CH:11]=[CH:12][C:13](=O)[NH:14][N:15]=2)[CH:5]=[CH:6][C:7]=1[O:8][CH3:9].P(Cl)(Cl)([Cl:19])=O>>[Br:1][C:2]1[CH:3]=[C:4]([C:10]2[N:15]=[N:14][C:13]([Cl:19])=[CH:12][CH:11]=2)[CH:5]=[CH:6][C:7]=1[O:8][CH3:9]

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 121965636-(3-Bromo-4-methoxyphenyl)-3(2H)-pyridazinone

生成物 1

HCID 122575033-(3-Bromo-4-methoxyphenyl)-6-chloropyridazine

実験手順

A suspension of 100 g. of 6-(3-bromo-4-methoxyphenyl)-3(2H)-pyridazinone [J. Heterocyclic Chem. 11, 775 (1974) ]in 150 ml. of phosphorus oxychloride is refluxed until a clear solution is obtained (approximately 5 hours). The solution is cooled and excess phosphorus oxychloride is removed under vacuum to give a brown solid which is triturated with ice water. The solid is collected by filtration and is recrystallized to afford 3-(3-bromo-4-methoxyphenyl)-6-chloropyridazine.

後処理

  1. additionA suspension of 100 g
  2. customis obtained (approximately 5 hours)
  3. temperatureThe solution is cooled
  4. customexcess phosphorus oxychloride is removed under vacuum
  5. customto give a brown solid which
  6. customis triturated with ice water
  7. filtrationThe solid is collected by filtration
  8. customis recrystallized

出典と根拠

ORDレコード
ord-262367b5719642fcbfb863d0973c56b2
出典データセット
uspto-grants-1978_09
特許番号
US04112095

反応ノート

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