Methyl 2-(3-amino-4-chlorophenoxy)acetate → HCID 68782003, 화합물

HRID 2266517노트

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HRID 2266517 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 68782003HCID 68782003, 화합물

시약·촉매·용매 1

HCID 962Water용매

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온도
100 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-8b9d164d7d1140c6ad3101a9ebb170a1
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07858640B2

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