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Methanesulfonic Acid → HCID 68783011、化合物

HRID 2266520
ノート
印刷プレビュー

反応式

HRID 2266520 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]([CH2:24][C:25]1[CH:30]=[CH:29][C:28]([Cl:31])=[CH:27][CH:26]=1)[C:20](=O)[CH2:21][CH3:22])C.CS(O)(=O)=O>C1(C)C=CC=CC=1>[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]([CH2:24][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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6395Methanesulfonic AcidHCID 66717604Methyl 2-(3-amino-4-chlorophenoxy)acetateHCID 66717606HCID 66717606、化合物

生成物 1

HCID 68783011HCID 68783011、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of (3-amino-4-chlorophenoxy)acetic acid methyl ester (0.53 g), 2-(4-chlorobenzyl)-3-oxopentanoic acid ethyl ester (0.66 g), methanesulfonic acid (0.032 mL) and toluene (20 mL) was heated at reflux for 20 hours. The mixture was cooled to room temperature and the solvent removed under reduced pressure. The residue was diluted with water, extracted with ethyl acetate and the combined extracts 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 (9:1 by volume) to afford title compound, 0.034 g

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 20 hours
  3. customthe solvent removed under reduced pressure
  4. additionThe residue was diluted with water
  5. extractionextracted with ethyl acetate
  6. dry with materialthe combined extracts dried over magnesium sulfate
  7. customThe solvent was removed under reduced pressure
  8. customthe residue purified by column chromatography on silica gel
  9. washeluting with a mixture of dichloromethane and ethyl acetate (9:1 by volume)

出典と根拠

ORDレコード
ord-7474ca0ee84c49a2a921ba068c56cba6
出典データセット
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07858640B2

反応ノート

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