Imidazole → HCID 68854444, 화합물

HRID 333022

반응식

HRID 333022 반응식
[Br:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1F)[C:5]#[N:6].[NH:11]1[CH:15]=[CH:14][N:13]=[CH:12]1.[H-].[Na+].O>CN(C)C=O>[Br:1][C:2]1[CH:3]=[C:4]([C:5]#[N:6])[CH:7]=[CH:8][C:9]=1[N:11]1[CH:15]=[CH:14][N:13]=[CH:12]1

참가 물질

6

반응물 4

HCID 795ImidazoleHCID 962WaterHCID 24758Sodium hydrideHCID 1235793-Bromo-4-fluorobenzonitrile

생성물 1

HCID 68854444HCID 68854444, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
100 °C

실험 절차

3-Bromo-4-fluorobenzonitrile (10.0 g, 50 mmol, 1 eq) and imidazole (5.1 g, 75 mmol, 1.5 eq) are dissolved in dimethylformamide (100 ml) and carefully admixed with sodium hydride (60% in mineral oil, 3.0 g, 75 mmol, 1.5 eq) under nitrogen at room temperature. The mixture is stirred at 100° C. for 4 hours. After cooling to room temperature, water (10 ml) is added and the mixture is evaporated to dryness. The residue is washed with water and petroleum ether and purified by column chromatography (silica gel, methyl tert-butyl ether/ethyl acetate gradient).

후처리

  1. temperatureAfter cooling to room temperature
  2. customthe mixture is evaporated to dryness
  3. washThe residue is washed with water and petroleum ether
  4. custompurified by column chromatography (silica gel, methyl tert-butyl ether/ethyl acetate gradient)

출처 및 근거

ORD 기록
ord-ebad00ea2dd64a198e30f0f28e1bf016
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08877937B2

연결된 노트

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