4-Methoxyphenol → HCID 24777539、化合物

HRID 1364457ノート

反応式

HRID 1364457 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([OH:9])=[CH:5][CH:4]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:17][C:18]1[CH:25]=[CH:24][CH:23]=[C:22]([N+:26]([O-:28])=[O:27])[C:19]=1[C:20]#[N:21]>CN(C)C=O.N1C=CC=CC=1.O>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([O:9][CH2:17][C:18]2[CH:25]=[CH:24][CH:23]=[C:22]([N+:26]([O-:28])=[O:27])[C:19]=2[C:20]#[N:21])=[CH:5][CH:4]=1

参加物

7

反応物 3

HCID 90154-MethoxyphenolHCID 11430Potassium CarbonateHCID 21928393HCID 21928393、化合物

生成物 1

HCID 24777539HCID 24777539、化合物収率 42.4%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 1049Pyridine溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
0 °C

実験手順

4-Methoxyphenol (0.1 g, 0.83 mmol) and potassium carbonate were added to a cooled (0° C.) and stirred solution of 2-bromomethyl-6-nitrobenzonitrile [W. T. Ashton and J. B. Hynes, J. Med. Chem, 16, 1233 (1973)] (0.2 g, 0.83 mmol) in dimethylformamide under nitrogen atmosphere. The reaction mixture was stirred at 0° C. for 1.5 hours, then diluted with pyridine (1.5 mL), water, stirred for 1 hour, filtered and dried. Purification by silica gel chromatography (50% hexanes in dichloromethane) yielded 100 mg of 2-(4-methoxyphenoxymethyl)-6-nitrobenzonitrile.

後処理

  1. stirringstirred for 1 hour
  2. filtrationfiltered
  3. customdried
  4. customPurification by silica gel chromatography (50% hexanes in dichloromethane)

出典と根拠

ORDレコード
ord-253376d2f3df408a9afbe6b965ecdb8f
出典データセット
uspto-grants-2011_02
特許番号
US07888366B2

反応ノート

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