Imidazole → HCID 59633930、化合物

HRID 1615087ノート

反応式

HRID 1615087 の反応式
[F:1][C:2]([F:11])([C:5]1[CH:10]=[CH:9][N:8]=[CH:7][CH:6]=1)[CH2:3][OH:4].N1C=CN=C1.[C:17]([Si:21]([CH3:24])([CH3:23])Cl)([CH3:20])([CH3:19])[CH3:18].O>CN(C=O)C>[Si:21]([O:4][CH2:3][C:2]([C:5]1[CH:10]=[CH:9][N:8]=[CH:7][CH:6]=1)([F:1])[F:11])([C:17]([CH3:20])([CH3:19])[CH3:18])([CH3:24])[CH3:23]

参加物

6

反応物 4

HCID 795ImidazoleHCID 962WaterHCID 28928tert-Butyldimethylsilyl chlorideHCID 596339072,2-Difluoro-2-(pyridin-4-yl)-ethanol2 回

生成物 1

HCID 59633930HCID 59633930、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 2,2-difluoro-2-(pyridin-4-yl)-ethanol (0.15 g) prepared in (2) in DMF (3.0 mL) were added imidazole (0.076 g) and tert-butyldimethylchlorosilane (0.15 g). The reaction mixture was stirred at RT for 2 hr. Water was added to the reaction mixture and the mixture was extracted with ethyl acetate. The organic layer was dried over MgSO4. The solvent was removed under reduced pressure. The residue was purified by silica gel chromatography (Developing solvent: ethyl acetate) to give the title compound.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. dry with materialThe organic layer was dried over MgSO4
  3. customThe solvent was removed under reduced pressure
  4. customThe residue was purified by silica gel chromatography (Developing solvent: ethyl acetate)

出典と根拠

ORDレコード
ord-5147dbfe2e2b4c199ae7c0790d789346
出典データセット
uspto-grants-2014_07
特許番号
US08765739B2

反応ノート

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