5-[2-(2,5-Dimethoxyphenyl)ethyl]-2-amino benzoic acid methylester → 5-[2-(2,5-Dimethoxyphenyl)ethyl]-2-methoxycarbonylamino Benzoic acid Methylester

HRID 1603535ノート

反応式

HRID 1603535 の反応式
[CH3:1][O:2][C:3](=[O:23])[C:4]1[CH:9]=[C:8]([CH2:10][CH2:11][C:12]2[CH:17]=[C:16]([O:18][CH3:19])[CH:15]=[CH:14][C:13]=2[O:20][CH3:21])[CH:7]=[CH:6][C:5]=1[NH2:22]>CN(C)C1C=CN=CC=1.ClCCl>[CH3:1][O:2][C:3](=[O:23])[C:4]1[CH:9]=[C:8]([CH2:10][CH2:11][C:12]2[CH:17]=[C:16]([O:18][CH3:19])[CH:15]=[CH:14][C:13]=2[O:20][CH3:21])[CH:7]=[CH:6][C:5]=1[NH:22][C:3]([O:2][CH3:1])=[O:23]

参加物

4

反応物 1

HCID 544614515-[2-(2,5-Dimethoxyphenyl)ethyl]-2-amino benzoic acid methylester

生成物 1

HCID 543092215-[2-(2,5-Dimethoxyphenyl)ethyl]-2-methoxycarbonylamino Benzoic acid Methylester

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒

実験手順

A mixture of 115 mg of 5-[2-(2,5-dimethoxyphenyl)ethyl]-2-amino benzoic acid methylester and 50 mg of 4-dimethylaminopyridine in 6 ml of dry dichloromethane is treated with 35 mg of methyl chloroformiate and stirred for 3 hours at room temperature. Then the mixture is poured onto aqueous pH7 buffer solution and extracted with ethyl acetate. The combined organic extracts are dried over magnesium sulfate and concentrated in vacuo. The crude product is purified by silica gel chromatography (cyclohexane/ethyl acetate=8/1) to yield the title compound as colourless crystals. mp: 80-82°.

後処理

  1. additionis treated with 35 mg of methyl chloroformiate
  2. extractionextracted with ethyl acetate
  3. dry with materialThe combined organic extracts are dried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe crude product is purified by silica gel chromatography (cyclohexane/ethyl acetate=8/1)

出典と根拠

ORDレコード
ord-dc304a7e6df74c3d8a8b730cbcae6740
出典データセット
uspto-grants-1999_11
特許番号
US05990116

反応ノート

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