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HCID 66717606, 화합물 → HCID 68783178, 화합물

HRID 2266546
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HRID 2266546 반응식
[CH3:1][O:2][C:3](=[O:14])[CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([F:12])=[C:8]([NH2:13])[CH:7]=1.C([O:17][C:18](=O)[CH:19]([CH2:24][C:25]1[CH:30]=[CH:29][C:28]([Cl:31])=[CH:27][CH:26]=1)[C:20](=O)[CH2:21][CH3:22])C>O>[CH3:1][O:2][C:3](=[O:14])[CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([F:12])=[C:8]2[C:7]=1[C:18](=[O:17])[C:19]([CH2:24][C:25]1[CH:26]=[CH:27][C:28]([Cl:31])=[CH:29][CH:30]=1)=[C:20]([CH2:21][CH3:22])[NH:13]2
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참가 물질

4

반응물 2

HCID 66717606HCID 66717606, 화합물HCID 66717607(3-Amino-4-fluorophenoxy)acetic acid methyl ester

생성물 1

HCID 68783178HCID 68783178, 화합물

시약·촉매·용매 1

HCID 962Water용매

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온도
120 °C

실험 절차

A mixture of (3-amino-4-fluorophenoxy)acetic acid methyl ester (1.9 g), 2-(4-chlorobenzyl)-3-oxopentanoic acid ethyl ester (0.95 g) and polyphosphoric acid (10 mL) was heated at 120° C. for 5 hours. The mixture was diluted with water, extracted with ethyl acetate and the combined extracts washed with saturated aqueous sodium chloride solution and saturated aqueous sodium hydrogen carbonate solution and then 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 dichloromethane and ethyl acetate (1:0 to 10:1 by volume) to afford title compound as a brown solid, 0.10 g.

후처리

  1. extractionextracted with ethyl acetate
  2. washthe combined extracts washed with saturated aqueous sodium chloride solution and saturated aqueous sodium hydrogen carbonate solution
  3. dry with materialdried over magnesium sulfate
  4. customThe solvent was removed under reduced pressure
  5. customthe residue purified by column chromatography on silica gel
  6. washeluting with a mixture of dichloromethane and ethyl acetate (1:0 to 10:1 by volume)

출처 및 근거

ORD 기록
ord-48d12264b4a242f19e9703a862b6cf82
출처 데이터셋
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07858640B2

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