Acrylic Acid → HCID 17244964、化合物

HRID 576739

反応式

HRID 576739 の反応式
[F:1][C:2]([F:17])([F:16])[C:3]1[CH:4]=[C:5]([NH:9]C2C=CC=CC=2)[CH:6]=[CH:7][CH:8]=1.[C:18]([OH:22])(=[O:21])[CH:19]=[CH2:20].[OH-].[Na+]>O>[F:1][C:2]([F:16])([F:17])[C:3]1[CH:4]=[C:5]([NH:9][CH2:20][CH2:19][C:18]([OH:22])=[O:21])[CH:6]=[CH:7][CH:8]=1

参加物

5

反応物 3

HCID 6581Acrylic AcidHCID 75483-(Trifluoromethyl)-N-phenylanilineHCID 14798Sodium Hydroxide

生成物 1

HCID 17244964HCID 17244964、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

To an aqueous solution of 3-trifluoromethylphenyl aniline (5.0 g) in water (15.0 ml) was added acrylic acid (3.2 ml) and the resulting mixture was stirred at 100° C. for one hour. The reaction mixture was basified with 5N aqueous sodium hydroxide solution and extracted with ethyl acetate (100 ml×2). The resulting organic layer was washed with saturated saline (50 ml), dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: chloroform/methanol) to afford 3-(3-trifluoromethylphenylamino)propionic acid (8.4 g).

後処理

  1. extractionextracted with ethyl acetate (100 ml×2)
  2. washThe resulting organic layer was washed with saturated saline (50 ml)
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (eluent: chloroform/methanol)

出典と根拠

ORDレコード
ord-26b75629e775465c8819f182137e5e1b
出典データセット
uspto-grants-2015_05
特許番号
US09040516B2

関連ノート

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