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Water → N-(4-Fluorophenyl)-N'-(4-{[2-(4-chlorobutyrylamino)-4-pyridyl]oxy}phenyl)urea

HRID 1010206
ノート
印刷プレビュー

反応式

HRID 1010206 の反応式
[Cl:1][CH2:2][CH2:3][CH2:4][C:5]([NH:7][C:8]1[CH:13]=[C:12]([O:14][C:15]2[CH:21]=[CH:20][C:18]([NH2:19])=[CH:17][CH:16]=2)[CH:11]=[CH:10][N:9]=1)=[O:6].[F:22][C:23]1[CH:28]=[CH:27][C:26]([N:29]=[C:30]=[O:31])=[CH:25][CH:24]=1.O1CCCC1.O>C(OCC)(=O)C>[F:22][C:23]1[CH:28]=[CH:27][C:26]([NH:29][C:30]([NH:19][C:18]2[CH:17]=[CH:16][C:15]([O:14][C:12]3[CH:11]=[CH:10][N:9]=[C:8]([NH:7][C:5](=[O:6])[CH2:4][CH2:3][CH2:2][Cl:1])[CH:13]=3)=[CH:21][CH:20]=2)=[O:31])=[CH:25][CH:24]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8028TetrahydrofuranHCID 709554-Fluorophenyl isocyanateHCID 579333274-([2-(4-Chlorobutyrylamino)-4-pyridyl]oxy)aniline

生成物 1

HCID 22936908N-(4-Fluorophenyl)-N'-(4-{[2-(4-chlorobutyrylamino)-4-pyridyl]oxy}phenyl)urea

試薬・触媒・溶媒 1

HCID 8857
Ethyl Acetate
溶媒

実験手順

4-{[2-(4-Chlorobutyrylamino)-4-pyridyl]oxy}aniline (100 mg), p-fluorophenyl isocyanate (0.037 ml) and tetrahydrofuran (3 ml) were stirred at room temperature for 25 minutes. Water and ethyl acetate were added to the reaction solution for extraction, NH type silica gel was added to the extract, the solvent was distilled off under reduced pressure and the reaction product was adsorbed onto the silica gel. The silica gel was charged into a dry column packed with NH type silica gel, and column purification was performed (hexane:ethyl acetate=1:1, followed by ethyl acetate and ethyl acetate:methanol=10:1). The solvent was distilled off under reduced pressure to obtain 56 mg of the target substance as a white solid.

後処理

  1. additionwas added to the extract
  2. distillationthe solvent was distilled off under reduced pressure
  3. additionThe silica gel was charged into a dry column
  4. custompacked with NH type silica gel, and column purification
  5. distillationThe solvent was distilled off under reduced pressure
  6. customto obtain 56 mg of the target substance as a white solid

出典と根拠

ORDレコード
ord-1f117204a9d5478b9fb41d84a09c50c8
出典データセット
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07973160B2

反応ノート

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