Methyl 2-(3-amino-4-chlorophenoxy)acetate → HCID 68780451、化合物

HRID 2266507ノート

反応式

HRID 2266507 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.C([O:17][C:18](=O)[CH:19]([CH2:23][C:24]1[CH:29]=[CH:28][C:27]([S:30]([CH3:33])(=[O:32])=[O:31])=[CH:26][C:25]=1[Cl:34])[C:20](=O)[CH3:21])C>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:18](=[O:17])[C:19]([CH2:23][C:24]1[CH:29]=[CH:28][C:27]([S:30]([CH3:33])(=[O:31])=[O:32])=[CH:26][C:25]=1[Cl:34])=[C:20]([CH3:21])[NH:13]2

参加物

4

反応物 2

HCID 66717604Methyl 2-(3-amino-4-chlorophenoxy)acetateHCID 687794542-(2-chloro-4-methanesulfonylbenzyl)-3-oxobutyric Acid Ethyl Ester

生成物 1

HCID 68780451HCID 68780451、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
130 °C

実験手順

A mixture of (3-amino-4-chlorophenoxy)acetic acid methyl ester (0.85 g), 2-(2-chloro-4-methanesulfonylbenzyl)-3-oxobutyric acid ethyl ester (2.1 g) and polyphosphoric acid (10 g) was heated at 130° 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 to afford title compound, 0.35 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

出典と根拠

ORDレコード
ord-19e91dc69e114470ae8f5c2a46c7ee82
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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