Phosphorus oxychloride → HCID 10384366、化合物

HRID 1647460ノート

反応式

HRID 1647460 の反応式
[C:1]([C:6]1[C:15](=O)[C:14]2[C:9](=[C:10]([CH2:17][O:18][C:19](=[O:26])[C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[CH:11]=[CH:12][CH:13]=2)[NH:8][CH:7]=1)(=[O:5])[CH:2]([CH3:4])[CH3:3].P(Cl)(Cl)([Cl:29])=O>>[C:1]([C:6]1[CH:7]=[N:8][C:9]2[C:14]([C:15]=1[Cl:29])=[CH:13][CH:12]=[CH:11][C:10]=2[CH2:17][O:18][C:19](=[O:26])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)(=[O:5])[CH:2]([CH3:4])[CH3:3]

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 10043403HCID 10043403、化合物

生成物 1

HCID 10384366HCID 10384366、化合物

実験手順

A solution of 3-isobutyryl-8-(benzoyloxymethyl)-4(1H)-quinolone (11.81 g, 29.9 mmol) in phosphoryl chloride (100 ml) was heated at reflux for 2.5 hours, then the excess phosphoryl chloride evaporated. Water was added and the product extracted into a mixture of dichloromethane and isopropyl alcohol. Drying and evaporation of the organic layer gave crude 3-isobutyryl-4-chloro-8-(benzoyloxymethyl)quinoline (12.0 g), contaminated with isopropyl alcohol. This was used without further purification.

後処理

  1. temperatureat reflux for 2.5 hours
  2. customthe excess phosphoryl chloride evaporated
  3. additionWater was added
  4. extractionthe product extracted into a mixture of dichloromethane and isopropyl alcohol
  5. customDrying
  6. customevaporation of the organic layer

出典と根拠

ORDレコード
ord-92aa79ba937f4fa896c79849779d1753
出典データセット
uspto-grants-1995_07
特許番号
US05432182

反応ノート

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