Imidazole → HCID 68854444、化合物

HRID 333022ノート

反応式

HRID 333022 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 68854444HCID 68854444、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-ebad00ea2dd64a198e30f0f28e1bf016
出典データセット
uspto-grants-2014_11
特許番号
US08877937B2

反応ノート

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