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

HRID 1603535노트

반응식

HRID 1603535 반응식
[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]

참가 물질

4

반응물 1

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

생성물 1

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

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

실험 절차

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°.

후처리

  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)

출처 및 근거

ORD 기록
ord-dc304a7e6df74c3d8a8b730cbcae6740
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05990116

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