1-Phenylpiperazine → HCID 23345032, 화합물

HRID 1856455노트

반응식

HRID 1856455 반응식
[O:1]1[CH2:19][CH:2]1[CH2:3][O:4][C:5]1[CH:6]=[C:7]([CH:13]2[CH2:17][NH:16][C:15](=[O:18])[CH2:14]2)[CH:8]=[CH:9][C:10]=1[O:11][CH3:12].[C:20]1([N:26]2[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]2)[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>CO>[CH3:12][O:11][C:10]1[CH:9]=[CH:8][C:7]([CH:13]2[CH2:17][NH:16][C:15](=[O:18])[CH2:14]2)=[CH:6][C:5]=1[O:4][CH2:3][CH:2]([OH:1])[CH2:19][N:29]1[CH2:30][CH2:31][N:26]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH2:27][CH2:28]1

참가 물질

4

반응물 2

HCID 70961-PhenylpiperazineHCID 23345057HCID 23345057, 화합물

생성물 1

HCID 23345032HCID 23345032, 화합물수율 61%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

15.5 millimoles of 4-[3-(2,3-epoxypropoxy)-4-methoxyphenyl]-2-pyrrolidone is dissolved in 50 ml. of methanol. After the addition of 15.5 mmol of 1-phenylpiperazine (95% strength), the reaction mixture is heated for 3 hours under reflux. After cooling of the reaction solution, the solvent is removed under vacuum at 40°. The residue is taken up in 50 ml. of 1N hydrochloric acid and extracted twice with 100 ml. of chloroform. The aqueous phase is adjusted to be alkaline with 2N sodium hydroxide solution and thereafter extracted three times with ethyl acetate. The combined ethyl acetate phase are washed with saturated sodium chloride solution, and the solvent, after drying over sodium sulfate, is distilled off under vacuum. The residue is recrystallized from ethanol, thus obtaining in a 61% yield 4-{4-methoxy-3-[3-(4-phenylpiperazin-1-yl)-2-hydroxypropoxy ]phenyl}-2-pyrrolidone, m.p. 143°-144°.

후처리

  1. temperaturethe reaction mixture is heated for 3 hours
  2. temperatureunder reflux
  3. temperatureAfter cooling of the reaction solution
  4. customthe solvent is removed under vacuum at 40°
  5. extractionof 1N hydrochloric acid and extracted twice with 100 ml
  6. extractionextracted three times with ethyl acetate
  7. washThe combined ethyl acetate phase are washed with saturated sodium chloride solution
  8. dry with materialthe solvent, after drying over sodium sulfate
  9. distillationis distilled off under vacuum
  10. customThe residue is recrystallized from ethanol

출처 및 근거

ORD 기록
ord-5f2da4f80fcf4f1c803468463369e82f
출처 데이터셋
uspto-grants-1980_08
특허 번호
US04219551

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