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Potassium Carbonate → methyl (E)-3-[4-(4-methylphenyl)thiophen-2-yl)acrylate

HRID 566022
ノート
印刷プレビュー

反応式

HRID 566022 の反応式
C/[C:2](=[CH:6]\[C:7]1[S:8][CH:9]=[C:10](Br)[CH:11]=1)/[C:3]([OH:5])=[O:4].B([O-])([O-])O[C:15]1[CH:20]=[CH:19][C:18]([CH3:21])=[CH:17][CH:16]=1.[C:24](=O)([O-])[O-].[K+].[K+]>C1(C)C(CCO)=CC=CC=1.O.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH3:21][C:18]1[CH:19]=[CH:20][C:15]([C:10]2[CH:11]=[C:7](/[CH:6]=[CH:2]/[C:3]([O:5][CH3:24])=[O:4])[S:8][CH:9]=2)=[CH:16][CH:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 866453334-Methylphenyl borateHCID 86756172methyl (E)-3-(4-bromothiophen-2-yl)acrylic acid

生成物 1

HCID 86756171methyl (E)-3-[4-(4-methylphenyl)thiophen-2-yl)acrylate収率 76.5%

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒
HCID 66602552
Toluene-ethanol water
溶媒

実験手順

Under argon atmosphere, a solution of methyl (E)-3-(4-bromothiophen-2-yl)acrylic acid (3.0 g), 4-methylphenyl borate (1.82 g) and potassium carbonate (3.36 g) in toluene-ethanol-water (120-12-12 ml) was stirred at room temperature for 1 hour. To the reaction mixture was added tetrakistriphenylphosphinepalladium (0.42 g), and the mixture was refluxed for 24 hours and cooled to room temperature. The organic layer was washed with saturated sodium chloride solution, dried with magnesium sulfate and concentrated under reduced pressure. The residue was separated and purified with column chromatography (ethyl acetate/hexane=1:9→1:5→1:2) to give methyl (E)-3-[4-(4-methylphenyl)thiophen-2-yl)acrylate (2.40 g) as pale yellow crystals.

後処理

  1. temperaturethe mixture was refluxed for 24 hours
  2. washThe organic layer was washed with saturated sodium chloride solution
  3. dry with materialdried with magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was separated
  6. custompurified with column chromatography (ethyl acetate/hexane=1:9→1:5→1:2)

出典と根拠

ORDレコード
ord-9488d397c6af4c089891a9a14d1ee4ff
出典データセット
uspto-grants-2001_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06172061B2

反応ノート

読み込み中…

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