Tetrabutylammonium Fluoride → 1-(1-Ethoxymethyl-4-hydroxymethyl-1H-imidazol-2-yl)ethanone

HRID 242372

反応式

HRID 242372 の反応式
[CH2:1]([O:3][CH2:4][N:5]1[CH:9]=[C:8]([CH2:10][O:11][Si](CC)(CC)CC)[N:7]=[C:6]1[C:19](=[O:21])[CH3:20])[CH3:2].[F-].C([N+](CCCC)(CCCC)CCCC)CCC>C1COCC1>[CH2:1]([O:3][CH2:4][N:5]1[CH:9]=[C:8]([CH2:10][OH:11])[N:7]=[C:6]1[C:19](=[O:21])[CH3:20])[CH3:2]

参加物

4

反応物 2

HCID 2724141Tetrabutylammonium FluorideHCID 710871971-[1-Ethoxymethyl-4-(triethylsilyloxymethyl)-1H-imidazol-2-yl]ethanone

生成物 1

HCID 682719271-(1-Ethoxymethyl-4-hydroxymethyl-1H-imidazol-2-yl)ethanone

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

The compound (520 mg) obtained in (4) was dissolved in THF (10 mL), followed by addition of tetrabutylammonium fluoride (TBAF, 1.0 M THF solution, 3.32 mL) under stirring, and the stirring was continued for 1 hour. The reaction solution was concentrated under reduced pressure, and the resulting residue was purified by flash chromatography (ethyl acetate/hexane=25%→100%) using amino column (product name: SNAP Cartridge KP-NH 55 g, manufactured by Biotage, Ltd.) to afford the title compound (288 mg).

後処理

  1. concentrationThe reaction solution was concentrated under reduced pressure
  2. customthe resulting residue was purified by flash chromatography (ethyl acetate/hexane=25%→100%)

出典と根拠

ORDレコード
ord-6d331297395d4da8b63cfab11b23c446
出典データセット
uspto-grants-2014_02
特許番号
US08653126B2

関連ノート

読み込み中…