Benzophenone → Benzimidazole

HRID 222870

反応式

HRID 222870 の反応式
S(=O)(=O)(O)O.[NH2:6][CH2:7][C:8]#[N:9].[C:10]([C:18]1C=CC=CC=1)(=O)[C:11]1C=CC=C[CH:12]=1.[CH3:24]CN(C(C)C)C(C)C>ClCCl>[N:9]1[C:8]2[CH:18]=[CH:10][CH:11]=[CH:12][C:7]=2[NH:6][CH:24]=1

参加物

5

反応物 3

HCID 3102BenzophenoneHCID 81531DiisopropylethylamineHCID 196971Aminoacetonitrile sulfate (1:1)

生成物 1

HCID 5798Benzimidazole収率 156,273.703%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a stirred solution of 2-aminoacetonitrile bisulfate (2.9 g, 0.013 mmol) in dichloromethane (50 mL) was added benzophenone (3.48 mL, 0.0208 mmol) followed by DIEA (4.53 mL, 0.026 mmol). After stirring 18 h, the dichloromethane solution was washed with water (50 mL), dried over sodium sulfate, filtered, and the filtrate concentrated under reduced pressure. The residue was purified on a flash silica gel column (hexanes:EtOAc, 1:1) to give 3 (2.40 g, 82%).

後処理

  1. washthe dichloromethane solution was washed with water (50 mL)
  2. dry with materialdried over sodium sulfate
  3. filtrationfiltered
  4. concentrationthe filtrate concentrated under reduced pressure
  5. customThe residue was purified on a flash silica gel column (hexanes:EtOAc, 1:1)

出典と根拠

ORDレコード
ord-135c9da0779349ac950e1ffb03afbab9
出典データセット
uspto-grants-2012_06
特許番号
US08207340B2

関連ノート

読み込み中…