Ethanol → N-(p-decylphenyl)-2,4,6-triphenylpyridinium bisulfate

HRID 652693ノート

反応式

HRID 652693 の反応式
[S:1](=[O:5])(=[O:4])([OH:3])[O-:2].[C:6]1([C:12]2[CH:17]=[C:16]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[CH:15]=[C:14]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)[O+]=2)[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.C(O)C.[CH2:33]([C:43]1[CH:49]=[CH:48][C:46]([NH2:47])=[CH:45][CH:44]=1)[CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH3:42].NC1C=CC=CC=1>C(#N)C>[S:1](=[O:3])(=[O:2])([OH:5])[O-:4].[CH2:33]([C:43]1[CH:44]=[CH:45][C:46]([N+:47]2[C:12]([C:6]3[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=3)=[CH:17][C:16]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[CH:15][C:14]=2[C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)=[CH:48][CH:49]=1)[CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH3:42]

参加物

6

反応物 4

HCID 702EthanolHCID 6115AnilineHCID 923094-DecylanilineHCID 117291982,4,6-Triphenylpyrylium Hydrogensulfate

生成物 1

HCID 20197780N-(p-decylphenyl)-2,4,6-triphenylpyridinium bisulfate

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

In a 500-ml round-bottom flask is placed 2.03 g (0.005 mole) of 2,4,6-triphenylpyrylium bisulfate. To this is added 150 ml of ethanol followed by 2.34 g (0.01 mole) of p-decylaniline. This mixture is refluxed for about 8 hours and allowed to cool. A quantity of the starting aniline precipitates and is removed by filtration. The ethanol is then removed to give a yellow waxy material which is washed with ether to give a white powder. This material is then dissolved in acetonitrile to cause the remaining aniline to precipitate. The acetonitrile is removed to give the desired product which is then rinsed with ether to remove any residual acetonitrile. The yield is 1.77 g (0.0028 mole) of 2,4,6-triphenylpyridinium bisulfate as confirmed by nuclear magnetic resonance (1H) and elemental analysis.

後処理

  1. customIn a 500-ml round-bottom flask is placed
  2. temperatureThis mixture is refluxed for about 8 hours
  3. temperatureto cool
  4. customA quantity of the starting aniline precipitates
  5. customis removed by filtration
  6. customThe ethanol is then removed
  7. customto give a yellow waxy material which
  8. washis washed with ether
  9. customto give a white powder
  10. customto precipitate
  11. customThe acetonitrile is removed

出典と根拠

ORDレコード
ord-637ebf6fb3d940c5879b4d0f036ded99
出典データセット
uspto-grants-1987_06
特許番号
US04672118

反応ノート

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