Acetic acid, 2-(triphenylphosphoranylidene)-, methyl ester → HCID 76563139, 화합물

HRID 548628노트

반응식

HRID 548628 반응식
[CH2:1]([N:8]1[CH2:12][CH2:11][C:10](=O)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C1(P(=[CH:33][C:34]([O:36][CH3:37])=[O:35])(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C1(C)C=CC=CC=1>[CH2:1]([N:8]1[CH2:12][CH2:11][C:10](=[CH:33][C:34]([O:36][CH3:37])=[O:35])[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 17453Acetic acid, 2-(triphenylphosphoranylidene)-, methyl esterHCID 698901-Benzyl-3-pyrrolidinone

생성물 1

HCID 76563139HCID 76563139, 화합물수율 61%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

1-benzylpyrrolidin-3-one a43 (8.75 g, 50 mmol, 1 eq) is dissolved in toluene (100 ml). Methyl (triphenylphosphoranylidene)acetate a44 (18.4 g, 55 mmol, 1.1 eq) is added and the mixture is refluxed for 60 h. The cold suspension is then filtered and the filtrate is concentrated to dryness. The crude product is purified by chromatography over silicagel (ethyl acetate/hexane 10/90) to afford 7.2 g of pure methyl (1-benzylpyrrolidin-3-ylidene)acetate a45.

후처리

  1. temperaturethe mixture is refluxed for 60 h
  2. filtrationThe cold suspension is then filtered
  3. concentrationthe filtrate is concentrated to dryness
  4. customThe crude product is purified by chromatography over silicagel (ethyl acetate/hexane 10/90)

출처 및 근거

ORD 기록
ord-9f034e1335e94b19b869bb49da883014
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07943605B2

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