Sulfuric acid magnesium salt (1:1) → 2-(4-(4-Methylpyridin-2-yl)-2-nitrobenzylidene)propionitrile

HRID 1060014ノート

反応式

HRID 1060014 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([C:8]2[CH:15]=[CH:14][C:11]([CH:12]=O)=[C:10]([N+:16]([O-:18])=[O:17])[CH:9]=2)[CH:3]=1.C1(P(C2C=CC=CC=2)(C2C=CC=CC=2)=[C:26]([CH3:29])[C:27]#[N:28])C=CC=CC=1.S([O-])([O-])(=O)=O.[Mg+2]>C1(C)C=CC=CC=1>[CH3:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([C:8]2[CH:15]=[CH:14][C:11]([CH:12]=[C:26]([CH3:29])[C:27]#[N:28])=[C:10]([N+:16]([O-:18])=[O:17])[CH:9]=2)[CH:3]=1

参加物

5

反応物 3

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 136931782-(Triphenylphosphoranylidene)propanenitrileHCID 186675944-(4-Methylpyridin-2-yl)-2-nitrobenzaldehyde

生成物 1

HCID 536430862-(4-(4-Methylpyridin-2-yl)-2-nitrobenzylidene)propionitrile収率 94.4%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A suspension of 4-(4-methylpyridin-2-yl)-2-nitrobenzaldehyde (203 mg) and 2-(triphenylphosphoranylidene)propionitrile (0.45 g) in toluene (10 ml) was refluxed for 3 hours. After cooling, to the reaction mixture were added magnesium sulfate and silica gel (10 g), and the suspension was stirred for 30 minutes. The solid was removed by filtration and washed with toluene (10 ml) three times. The combined filtrate was evaporated under reduced pressure to give 2-(4-(4-methylpyridin-2-yl)-2-nitrobenzylidene)propionitrile (221 mg) as a mixture of regioisomers.

後処理

  1. temperaturewas refluxed for 3 hours
  2. temperatureAfter cooling, to the reaction mixture
  3. customThe solid was removed by filtration
  4. washwashed with toluene (10 ml) three times
  5. customThe combined filtrate was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-f5b6968ef04c480daa596c4388ac74e5
出典データセット
uspto-grants-2003_02
特許番号
US06521643B1

反応ノート

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