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

HRID 653405

반응식

HRID 653405 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 1662802-(1-Piperazinyl)-4-phenylquinolone수율 91.1%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0fab2c8e58474efeb2d1022ba0ffa8ac
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04677107

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