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Tetrahydrofuran → 2-(2,4-Difluorophenyl)-1-(3-ethoxyphenyl)-1H-imidazole-4-carboxylic acid

HRID 2356596
ノート
印刷プレビュー

反応式

HRID 2356596 の反応式
[CH2:1]([O:3][C:4]1[CH:5]=[C:6]([NH:10][C:11]([C:13]2[CH:18]=[CH:17][C:16]([F:19])=[CH:15][C:14]=2[F:20])=[NH:12])[CH:7]=[CH:8][CH:9]=1)[CH3:2].C[Si]([N-][Si](C)(C)C)(C)C.[Na+].C([O:33][C:34]1C=C(C=[CH:39][CH:40]=1)N)C.FC1C=C(F)C=CC=1C#N.[O:51]1CCCC1>[Cl-].[Na+].O.ClCCl>[CH2:1]([O:3][C:4]1[CH:5]=[C:6]([N:10]2[CH:39]=[C:40]([C:34]([OH:33])=[O:51])[N:12]=[C:11]2[C:13]2[CH:18]=[CH:17][C:16]([F:19])=[CH:15][C:14]=2[F:20])[CH:7]=[CH:8][CH:9]=1)[CH3:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 8028TetrahydrofuranHCID 121203-EthoxyanilineHCID 775452,4-DifluorobenzonitrileHCID 2724254Sodium bis(trimethylsilyl)amideHCID 178466610HCID 178466610、化合物

生成物 1

HCID 534142232-(2,4-Difluorophenyl)-1-(3-ethoxyphenyl)-1H-imidazole-4-carboxylic acid

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 57417360Sodium chloride; water溶媒

反応条件

温度
-78 °C

実験手順

N-(3-Ethoxyphenyl)-2,4-difluorobenzenecarboximidamide To a solution of 2.2 ml (4.4 mmol) of 2.0 M (in tetrahydrofuran) sodium bis(trimethylsilyl)amide in 10 mL of tetrahydrofuran at ambient temperature was added 0.52 mL (4.0 mmol) of 3-ethoxyaniline and the resulting solution was stirred for 20 min. The reaction mixture was cooled to −78° C. and then was added 0.57 ml (4.0 mmol) of 2,4-difluorobenzonitrile. The resulting mixture was stirred from −78° C. to ambient temperature for 5 hrs and then poured into brine (25 mL) and dichloromethane (50 mL). The organic layer was separated and the aqueous layer was extracted with dichloromethane (25 mL). The combined organic layers were dried over sodium sulfate, filtered and concentrated in vacuo. Flash chromatography on a Biotage Horizon® system (silica gel, 0 to 50% ethyl acetate in hexanes gradient) gave the title compound as a yellow oil. LC/MS 277.2 (M+1).

後処理

  1. stirringThe resulting mixture was stirred from −78° C. to ambient temperature for 5 hrs
  2. customThe organic layer was separated
  3. extractionthe aqueous layer was extracted with dichloromethane (25 mL)
  4. dry with materialThe combined organic layers were dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-388353a10fa74a2a877748f71b739f27
出典データセット
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07759352B2

反応ノート

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