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2,5-Dimethoxytetrahydrofuran → 2-{4-[1-[4-(1H-pyrrol-1-yl)phenyl]-3-(trifluoromethyl)-1H-pyrazol-5-yl]phenyl}ethyl acetate

HRID 351260
ノート
印刷プレビュー

反応式

HRID 351260 の反応式
[C:1]([O:4][CH2:5][CH2:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[N:17]([C:18]3[CH:23]=[CH:22][C:21]([NH2:24])=[CH:20][CH:19]=3)[N:16]=[C:15]([C:25]([F:28])([F:27])[F:26])[CH:14]=2)=[CH:9][CH:8]=1)(=[O:3])[CH3:2].CO[CH:31]1[CH2:35][CH2:34][CH:33](OC)O1>CC(O)=O>[C:1]([O:4][CH2:5][CH2:6][C:7]1[CH:8]=[CH:9][C:10]([C:13]2[N:17]([C:18]3[CH:23]=[CH:22][C:21]([N:24]4[CH:31]=[CH:35][CH:34]=[CH:33]4)=[CH:20][CH:19]=3)[N:16]=[C:15]([C:25]([F:26])([F:28])[F:27])[CH:14]=2)=[CH:11][CH:12]=1)(=[O:3])[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

4

反応物 2

HCID 790982,5-Dimethoxytetrahydrofuran2 回HCID 210907062-{4-[1-(4-aminophenyl)-3-(trifluoro-methyl)-1H-pyrazol-5-yl]phenyl}ethyl acetate

生成物 1

HCID 210907052-{4-[1-[4-(1H-pyrrol-1-yl)phenyl]-3-(trifluoromethyl)-1H-pyrazol-5-yl]phenyl}ethyl acetate収率 72.8%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
50 °C

実験手順

A mixture of 2-{4-[1-(4-aminophenyl)-3-(trifluoromethyl)-1H-pyrazol-5-yl]phenyl}ethyl acetate 165.6 mg and 2,5-dimethoxytetrahydrofuran 112 mg in AcOH 3 ml was stirred at 50° C. for 3 hours. 2,5-Dimethoxytetrahydrofuran 0.22 ml was added and the mixture was stirred at 50° C. for 2 hours. The mixture was partitioned between ethyl acetate and H2O. The organic layer was washed with saturated aqueous sodium bicarbonate solution and saturated aqueous sodium chloride solution, dried over magnesium sulfate, and concentrated in vacuo. The residue was purified by preparative thin layer silica gel chromatography developed by AcOEt/n-hexane=20%. The separated silica gel was extracted with 10% MeOH/CHCl3 and the solvent was evaporated in vacuo to give 2-{4-[1-[4-(1H-pyrrol-1-yl)phenyl]-3-(trifluoromethyl)-1H-pyrazol-5-yl]phenyl}ethyl acetate 136.1 mg as an oil.

後処理

  1. stirringthe mixture was stirred at 50° C. for 2 hours
  2. customThe mixture was partitioned between ethyl acetate and H2O
  3. washThe organic layer was washed with saturated aqueous sodium bicarbonate solution and saturated aqueous sodium chloride solution
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by preparative thin layer silica gel chromatography
  7. extractionThe separated silica gel was extracted with 10% MeOH/CHCl3
  8. customthe solvent was evaporated in vacuo

出典と根拠

ORDレコード
ord-fee74556b62b4488bade5b3d017dce4f
出典データセット
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07183306B2

反応ノート

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