Phosphorus oxychloride → 3-Chloro-6-(3-methylpentan-3-yl)pyridazine

HRID 434586ノート

反応式

HRID 434586 の反応式
[CH2:1]([C:3]([C:7]1[CH:8]=[CH:9][C:10](=O)[NH:11][N:12]=1)([CH3:6])[CH2:4][CH3:5])[CH3:2].P(Cl)(Cl)([Cl:16])=O>>[Cl:16][C:10]1[N:11]=[N:12][C:7]([C:3]([CH2:4][CH3:5])([CH3:6])[CH2:1][CH3:2])=[CH:8][CH:9]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 131886886-(3-Methylpentan-3-yl)pyridazin-3(2H)-one

生成物 1

HCID 131886893-Chloro-6-(3-methylpentan-3-yl)pyridazine

実験手順

To 34 g. of 6-(1-ethyl-1-methylpropyl)pyridazin-3-one was added 175 ml. of phosphorus oxychloride, and the mixture was stirred under reflux for 30 minutes. It was then cooled, excess phosphorus oxychloride was removed under vacuum, and the residual oil was poured into ice water. The residue was made basic to pH 9 with ammonia, and triturated. The aqueous mixture so prepared was extracted with two one-liter portions of diethyl ether, and the combined organics were dried and evaporated under vacuum to obtain 35 g. of the desired product, identified by mass spectroscopy, which showed a molecular ion having a weight of 198.

後処理

  1. temperatureunder reflux for 30 minutes
  2. temperatureIt was then cooled
  3. customexcess phosphorus oxychloride was removed under vacuum
  4. additionthe residual oil was poured into ice water
  5. customtriturated
  6. customThe aqueous mixture so prepared
  7. extractionwas extracted with two one-liter portions of diethyl ether
  8. customthe combined organics were dried
  9. customevaporated under vacuum
  10. customto obtain 35 g

出典と根拠

ORDレコード
ord-ca3603cffb6a426cbefdf2bf71744a35
出典データセット
uspto-grants-1983_08
特許番号
US04398044

反応ノート

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