Benzophenone → Benzimidazole

HRID 730327

반응식

HRID 730327 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 5798Benzimidazole수율 156,273.703%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-0e81b14c40264ccfa4abbea20ac7b045
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07582668B2

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