Water → 2-(1-Piperazinyl)-4-phenylquinolone

HRID 653405

反応式

HRID 653405 の反応式
Cl[C:2]1[CH:11]=[C:10]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.[NH:18]1[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]1.O>C1(C)C=CC=CC=1>[N:18]1([C:2]2[CH:11]=[C:10]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[C:9]3[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=3)[N:3]=2)[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]1

参加物

5

反応物 3

HCID 962WaterHCID 4837PiperazineHCID 23066872-Chloro-4-phenylquinoline

生成物 1

HCID 1662802-(1-Piperazinyl)-4-phenylquinolone収率 91.1%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A solution of 2-chloro-4-phenylquinoline (4.0 g) and anhydrous piperazine (8.0 g) in toluene (4 ml) is heated under reflux for 5 hours. To the reaction mixture is added water and the resulting mixture is extracted with ethyl acetate. The extracts are dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue is chromatographed on silica gel (40 g) using chloroform as an eluent. Fractions containing the title compound are pooled and concentrated to give the title compound (4.4 g), m.p. 133°-134° C.

後処理

  1. temperatureunder reflux for 5 hours
  2. extractionthe resulting mixture is extracted with ethyl acetate
  3. dry with materialThe extracts are dried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue is chromatographed on silica gel (40 g)
  6. additionFractions containing the title compound
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-0fab2c8e58474efeb2d1022ba0ffa8ac
出典データセット
uspto-grants-1987_06
特許番号
US04677107

関連ノート

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