Methyl 2-(3-amino-4-chlorophenoxy)acetate → HCID 68782003、化合物

HRID 2266517ノート

反応式

HRID 2266517 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.[Cl:15][C:16]1[CH:29]=[C:28]([S:30]([CH3:33])(=[O:32])=[O:31])[CH:27]=[CH:26][C:17]=1[CH2:18][CH:19]([C:23](=O)[CH3:24])[C:20](=O)[CH3:21]>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:20]([CH3:21])=[C:19]([CH2:18][C:17]1[CH:26]=[CH:27][C:28]([S:30]([CH3:33])(=[O:32])=[O:31])=[CH:29][C:16]=1[Cl:15])[C:23]([CH3:24])=[N:13]2

参加物

4

反応物 2

HCID 66717604Methyl 2-(3-amino-4-chlorophenoxy)acetateHCID 687834363-(2-Chloro-4-methanesulfonylbenzyl)pentane-2,4-dione

生成物 1

HCID 68782003HCID 68782003、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), 3-(2-chloro-4-methanesulfonylbenzyl)pentane-2,4-dione (0.5 g) and polyphosphoric acid (5.0 g) was heated at 100° C. for 3.5 hours. The mixture was cooled to room temperature, diluted with water and extracted with ethyl acetate. The combined extracts were washed with water and saturated aqueous sodium chloride solution and dried over magnesium sulfate. The solvent was removed under reduced pressure and the residue purified by column chromatography on silica gel, eluting with a mixture of ethyl acetate and cyclohexane (2:8 to 3:7 by volume) to afford title compound as a pale yellow waxy solid, 0.36 g.

後処理

  1. temperatureThe mixture was cooled to room temperature
  2. extractionextracted with ethyl acetate
  3. washThe combined extracts were washed with water and saturated aqueous sodium chloride solution
  4. dry with materialdried over magnesium sulfate
  5. customThe solvent was removed under reduced pressure
  6. customthe residue purified by column chromatography on silica gel
  7. washeluting with a mixture of ethyl acetate and cyclohexane (2:8 to 3:7 by volume)

出典と根拠

ORDレコード
ord-8b9d164d7d1140c6ad3101a9ebb170a1
出典データセット
uspto-grants-2010_12
特許番号
US07858640B2

反応ノート

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