Acetic acid, 2-(triphenylphosphoranylidene)-, methyl ester → HCID 76563139、化合物

HRID 548628ノート

反応式

HRID 548628 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 76563139HCID 76563139、化合物収率 61%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-9f034e1335e94b19b869bb49da883014
出典データセット
uspto-grants-2011_05
特許番号
US07943605B2

反応ノート

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