3-Chlorothiophenol → 3-[[(3-Chlorophenyl)thio]methyl]-2-pyridinecarbonitrile

HRID 1647249ノート

反応式

HRID 1647249 の反応式
C[O-].[Na+].[Cl:4][C:5]1[CH:6]=[C:7]([SH:11])[CH:8]=[CH:9][CH:10]=1.[C:12]([C:14]1[C:19]([CH2:20]Br)=[CH:18][CH:17]=[CH:16][N:15]=1)#[N:13]>CO>[C:12]([C:14]1[C:19]([CH2:20][S:11][C:7]2[CH:8]=[CH:9][CH:10]=[C:5]([Cl:4])[CH:6]=2)=[CH:18][CH:17]=[CH:16][N:15]=1)#[N:13]

参加物

5

反応物 3

HCID 162573-ChlorothiophenolHCID 103754503-(Bromomethyl)pyridine-2-carbonitrileHCID 10942334Sodium Methoxide

生成物 1

HCID 152802283-[[(3-Chlorophenyl)thio]methyl]-2-pyridinecarbonitrile

試薬・触媒・溶媒 1

HCID 887Methanol溶媒3 回

実験手順

To a stirred, cloudy solution of sodium methoxide (14.7 g, 0.27 mol) in methanol (450 mL), contained in a water bath, add a solution of 3-chlorothiophenol (39.5 g, 0.27 mol) in methanol (95 mL). To the resultant solution add a solution of 2-cyano-3-(bromomethyl)pyridine (48.9 g, 0.25 mol) in methanol (195 mL), and stir the reaction mixture at room temperature for 1 h. Concentrate the reaction mixture under reduced pressure, add 500 mL of ether to the residue, stir, and filter to remove the sodium bromide. Evaporate ether under reduced pressure to obtain the title compound as an amber oil, which may be used without further purification.

後処理

  1. concentrationConcentrate the reaction mixture under reduced pressure
  2. additionadd 500 mL of ether to the residue
  3. stirringstir
  4. filtrationfilter
  5. customto remove the sodium bromide

出典と根拠

ORDレコード
ord-eccfa7eb6d1249b5856b54ee2c4c26cc
出典データセット
uspto-grants-1995_07
特許番号
US05430032

反応ノート

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