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3-Fluoro-4-methoxymethoxy-5-vinylbenzoic acid methyl ester → 3-Fluoro-4-hydroxy-5-vinylbenzoic acid methyl ester

HRID 423246
ノート
印刷プレビュー

反応式

HRID 423246 の反応式
[CH3:1][O:2][C:3](=[O:17])[C:4]1[CH:9]=[C:8]([CH:10]=[CH2:11])[C:7]([O:12]COC)=[C:6]([F:16])[CH:5]=1>C1COCC1.C(OCC)(=O)C>[CH3:1][O:2][C:3](=[O:17])[C:4]1[CH:9]=[C:8]([CH:10]=[CH2:11])[C:7]([OH:12])=[C:6]([F:16])[CH:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 586297733-Fluoro-4-methoxymethoxy-5-vinylbenzoic acid methyl ester

生成物 1

HCID 586297433-Fluoro-4-hydroxy-5-vinylbenzoic acid methyl ester収率 80.1%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A solution of 3-fluoro-4-methoxymethoxy-5-vinylbenzoic acid methyl ester (185 mg) in THF (2 mL)-3N hydrochloric acid (1 mL) was stirred at 60° C. for 3 hours under heating. The mixture was allowed to stand for cooling down to room temperature, diluted with ethyl acetate, washed successively with water, saturated aqueous sodium bicarbonate and saturated brine, dried over anhydrous sodium sulfate, and concentrated in vacuo. The residue was purified by column chromatography on silica gel (hexane:ethyl acetate=9:1, v/v) to give the title compound (121 mg). (In the above, THF is tetrahydrofuran).

後処理

  1. temperatureunder heating
  2. washwashed successively with water, saturated aqueous sodium bicarbonate and saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by column chromatography on silica gel (hexane

出典と根拠

ORDレコード
ord-27ad0bce5f344dfa8c0da8c62a23a189
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08101774B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート