Acetic acid, 2-(triphenylphosphoranylidene)-, methyl ester → Methyl 3-(3-bromophenyl)prop-2-enoate

HRID 565976

反応式

HRID 565976 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=O.[CH3:10][O:11][C:12]([CH:14]=P(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)=[O:13]>C1(C)C=CC=CC=1>[Br:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=[CH:14][C:12]([O:11][CH3:10])=[O:13]

参加物

4

反応物 2

HCID 17453Acetic acid, 2-(triphenylphosphoranylidene)-, methyl esterHCID 765833-Bromobenzaldehyde

生成物 1

HCID 610698Methyl 3-(3-bromophenyl)prop-2-enoate収率 82.1%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a mixture of 3-bromobenzaldehyde (10 g) and methoxy-carbonylmethylenetriphenylphosphine (20 g) was added toluene (150 ml), and the mixture was refluxed under nitrogen atmosphere for 2 hours. The solvent was evaporated, and the organic layer was washed with water and saturated sodium chloride solution, and dried with anhydrous magnesium sulfate. Under reduced pressure, the solvent was evaporated, and the residue was purified with silica gel column (ethyl acetate/hexane) to give methyl 3-bromocinnamate (10.7 g) as colorless crystals.

後処理

  1. temperaturethe mixture was refluxed under nitrogen atmosphere for 2 hours
  2. customThe solvent was evaporated
  3. washthe organic layer was washed with water and saturated sodium chloride solution
  4. dry with materialdried with anhydrous magnesium sulfate
  5. customUnder reduced pressure, the solvent was evaporated
  6. customthe residue was purified with silica gel column (ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-65c2babea8e342569f6c0af4febad92b
出典データセット
uspto-grants-2001_01
特許番号
US06172061B2

関連ノート

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