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Trimethylaluminum → 3-[[1-(4-Fluorophenyl)-5-isopropylpyrazol-4-yl]amino]-3-[2-methyl-4-(trifluoromethyl)imidazol-1-yl]propan-1-ol

HRID 522317
ノート
印刷プレビュー

反応式

HRID 522317 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:12]([CH:13]([CH3:15])[CH3:14])=[C:11]([NH2:16])[CH:10]=[N:9]2)=[CH:4][CH:3]=1.[CH3:17][C:18]1[N:19]([CH:27]2[CH2:31][CH2:30][O:29]C2=O)[CH:20]=[C:21]([C:23]([F:26])([F:25])[F:24])[N:22]=1.C[Al](C)C>[OH-].[NH4+]>[F:1][C:2]1[CH:3]=[CH:4][C:5]([N:8]2[C:12]([CH:13]([CH3:14])[CH3:15])=[C:11]([NH:16][CH:27]([N:19]3[CH:20]=[C:21]([C:23]([F:25])([F:26])[F:24])[N:22]=[C:18]3[CH3:17])[CH2:31][CH2:30][OH:29])[CH:10]=[N:9]2)=[CH:6][CH:7]=1
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

5

反応物 3

HCID 16682925TrimethylaluminumHCID 664257241-(4-Fluorophenyl)-5-isopropyl-pyrazol-4-amineHCID 867230313-[2-Methyl-4-(trifluoromethyl)imidazol-1-yl]tetrahydrofuran-2-one

生成物 1

HCID 867230303-[[1-(4-Fluorophenyl)-5-isopropylpyrazol-4-yl]amino]-3-[2-methyl-4-(trifluoromethyl)imidazol-1-yl]propan-1-ol収率 24%

試薬・触媒・溶媒 1

HCID 14923
Ammonium Hydroxide
溶媒

反応条件

温度
55 °C

実験手順

A mixture of 1-(4-fluorophenyl)-5-isopropyl-pyrazol-4-amine (0.070 g, 0.32 mmol), 3-[2-methyl-4-(trifluoromethyl)imidazol-1-yl]tetrahydrofuran-2-one (0.070 g, 0.30 mmol) and AlMe3 (0.50 mL, 1.0 mmol, 2 M/toluene) was heated at 55° C. for 1.5 hrs. The mixture was then cooled to room temperature, diluted with aqueous ammonium hydroxide, and extracted with EtOAc. The organic layer was separated, dried over anhydrous sodium sulfate, concentrated in vacuo, and purified by flash chromatography (SiO2, 0˜20% MeOH/CH2Cl2 gradient elution) to give 3-[[1-(4-fluorophenyl)-5-isopropylpyrazol-4-yl]amino]-3-[2-methyl-4-(trifluoromethyl)imidazol-1-yl]propan-1-ol (0.030 g, 24%).

後処理

  1. temperatureThe mixture was then cooled to room temperature
  2. extractionextracted with EtOAc
  3. customThe organic layer was separated
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated in vacuo
  6. custompurified by flash chromatography (SiO2, 0˜20% MeOH/CH2Cl2 gradient elution)

出典と根拠

ORDレコード
ord-d3fe0f7fe50147b5bbd43efbdbda4cba
出典データセット
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09328116B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート