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(3-Amino-4-fluorophenoxy)acetic acid methyl ester → [2-ethyl-8-fluoro-3-(4-fluorobenzyl)-4-oxo-1,4-dihydroquinolin-5-yloxy]acetic Acid Methyl Ester

HRID 2266549
ノート
印刷プレビュー

反応式

HRID 2266549 の反応式
[CH3:1][O:2][C:3](=[O:14])[CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([F:12])=[C:8]([NH2:13])[CH:7]=1.C[O:16][C:17](=O)[CH:18]([CH2:23][C:24]1[CH:29]=[CH:28][C:27]([F:30])=[CH:26][CH:25]=1)[C:19](=O)[CH2:20][CH3:21]>O1CCOCC1>[CH3:1][O:2][C:3](=[O:14])[CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([F:12])=[C:8]2[C:7]=1[C:17](=[O:16])[C:18]([CH2:23][C:24]1[CH:25]=[CH:26][C:27]([F:30])=[CH:28][CH:29]=1)=[C:19]([CH2:20][CH3:21])[NH:13]2
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 66717607(3-Amino-4-fluorophenoxy)acetic acid methyl esterHCID 687831752-(4-fluorobenzyl)-3-oxopentanoic Acid Methyl Ester

生成物 1

HCID 68783191[2-ethyl-8-fluoro-3-(4-fluorobenzyl)-4-oxo-1,4-dihydroquinolin-5-yloxy]acetic Acid Methyl Ester

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
130 °C

実験手順

A mixture of (3-amino-4-fluorophenoxy)acetic acid methyl ester (0.80 g), 2-(4-fluorobenzyl)-3-oxopentanoic acid methyl ester (1.0 g), polyphosphoric acid (10 g) and dioxane (10 mL) was heated at 130° C. for 17 hours. The mixture was cooled to room temperature and partitioned between ethyl acetate and water. The aqueous phase was extracted with ethyl acetate and the combined organic phases washed with saturated aqueous sodium chloride solution and dried over magnesium sulfate. The solvent was removed under reduced pressure to afford title compound, 1.5 g.

後処理

  1. temperatureThe mixture was cooled to room temperature
  2. custompartitioned between ethyl acetate and water
  3. extractionThe aqueous phase was extracted with ethyl acetate
  4. washthe combined organic phases washed with saturated aqueous sodium chloride solution
  5. dry with materialdried over magnesium sulfate
  6. customThe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-57bb94635cdd481fb547286d172bb295
出典データセット
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07858640B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート