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Methyl 2-(3-amino-4-chlorophenoxy)acetate → HCID 68783790、化合物

HRID 2266526
ノート
印刷プレビュー

反応式

HRID 2266526 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]([Cl:12])=[C:8]([NH2:13])[CH:7]=1.[CH3:15][S:16]([C:19]1[CH:34]=[CH:33][C:22]([CH2:23][CH:24]([C:29](=O)[CH2:30][CH3:31])[C:25](=O)[CH2:26][CH3:27])=[CH:21][CH:20]=1)(=[O:18])=[O:17]>O>[CH3:1][O:2][C:3](=[O:14])[CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([Cl:12])=[C:8]2[C:7]=1[C:25]([CH2:26][CH3:27])=[C:24]([CH2:23][C:22]1[CH:21]=[CH:20][C:19]([S:16]([CH3:15])(=[O:18])=[O:17])=[CH:34][CH:33]=1)[C:29]([CH2:30][CH3:31])=[N: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 66717604Methyl 2-(3-amino-4-chlorophenoxy)acetateHCID 68784837HCID 68784837、化合物

生成物 1

HCID 68783790HCID 68783790、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

A mixture of (3-amino-4-chlorophenoxy)acetic acid methyl ester (0.35 g), 4-(4-methanesulfonylbenzyl)heptane-3,5-dione (0.49 g) and polyphosphoric acid (5.0 g) was heated at 100° C. for 2 hours. The mixture was cooled to room temperature, diluted with water and extracted with ethyl acetate. The combined extracts were dried over magnesium sulfate and the solvent removed under reduced pressure. The residue was purified by column chromatography on silica gel, eluting with a mixture of dichloromethane and methanol (99.5:0.5 by volume) to afford title compound, 0.20 g.

後処理

  1. temperatureThe mixture was cooled to room temperature
  2. extractionextracted with ethyl acetate
  3. dry with materialThe combined extracts were dried over magnesium sulfate
  4. customthe solvent removed under reduced pressure
  5. customThe residue was purified by column chromatography on silica gel
  6. washeluting with a mixture of dichloromethane and methanol (99.5:0.5 by volume)

出典と根拠

ORDレコード
ord-cf8df8233742428fbf7b10289a4131d7
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