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Methyl 4-Formylbenzoate → Methyl 4-ethenylbenzoate

HRID 428714
ノート
印刷プレビュー

反応式

HRID 428714 の反応式
[CH2:1]([Li])CCC.[CH:6]([C:8]1[CH:17]=[CH:16][C:11]([C:12]([O:14][CH3:15])=[O:13])=[CH:10][CH:9]=1)=O>CCOCC.[Br-].C[P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[CH3:15][O:14][C:12](=[O:13])[C:11]1[CH:16]=[CH:17][C:8]([CH:6]=[CH2:1])=[CH:9][CH:10]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 15294Methyl 4-FormylbenzoateHCID 178418339Butyllithium

生成物 1

HCID 583124Methyl 4-ethenylbenzoate

試薬・触媒・溶媒 2

HCID 74505Methyltriphenyliphosphonium bromide触媒HCID 3283Diethyl Ether溶媒

実験手順

To a stirred solution of n-butyllithium (4 mL, 2,5 M solution in hexane, 10 mmol) (Aldrich) in ether (30 mL) was added methyltriphenylphosphonium bromide (3.57 g, 10 mmol) (Aldrich) over a period of 5 min. The reaction mixture was stirred for 4 h at room temperature. To the resulting orange solution was added methyl 4-formylbenzoate (1.54 mL, 10 mmol) dropwise. The solution became colorless, and a white precipitate separated. The mixture was then heated to reflux and immediately allowed to cool to room temperature. The precipitate was removed by filtration. The resulting precipitate was washed with ether, and the combined ethereal filtrates were washed with water until neutral and then dried over anhydrous MgSO4. The solvent was removed and the residue, 4-ethenyl-benzoic acid methyl ester, was used in the next reaction without further purification.

後処理

  1. customa white precipitate separated
  2. temperatureThe mixture was then heated
  3. temperatureto reflux
  4. temperatureto cool to room temperature
  5. customThe precipitate was removed by filtration
  6. washThe resulting precipitate was washed with ether
  7. washthe combined ethereal filtrates were washed with water until neutral and
  8. dry with materialthen dried over anhydrous MgSO4
  9. customThe solvent was removed
  10. customthe residue, 4-ethenyl-benzoic acid methyl ester, was used in the next reaction without further purification

出典と根拠

ORDレコード
ord-8693104f274b45b6a1977f38b376508b
出典データセット
uspto-grants-2001_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06313310B1

反応ノート

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