4-Methylbenzaldehyde → p-Tolunitrile

HRID 53403

反応式

HRID 53403 の反応式
S([O-])([O-])(=O)=O.[Na+].[Na+].[CH3:8][C:9]1[CH:16]=[CH:15][C:12]([CH:13]=O)=[CH:11][CH:10]=1.S([O-])([O-])(=O)=O.O[NH3+:23].O[NH3+]>>[CH3:8][C:9]1[CH:16]=[CH:15][C:12]([C:13]#[N:23])=[CH:11][CH:10]=1

参加物

4

反応物 3

HCID 77254-MethylbenzaldehydeHCID 24436Sodium SulfateHCID 24846Hydroxylamine sulfate

生成物 1

HCID 7724p-Tolunitrile

反応条件

温度
80 °C

実験手順

With stirring (20 rpm), a turbine dryer is charged at room temperature with 8000 parts by weight of anhydrous sodium sulfate, 1602 parts by weight of 4-methylbenzaldehyde and 1149 parts by weight of hydroxylammonium sulfate. Following evacuation to 35 mbar, the mixture is heated to 80° C. and stirred at this temperature for 21/2 hours. It is subsequently heated at 125° C. at a pressure of 80 mbar and held for 10 minutes; the pressure is then reduced to 60 mbar and held for a further 20 minutes, during which a total of about 480 parts by weight of water are removed by distillation. The distillation of the nitrile is initiated and controlled by successive reduction of the pressure to 10 mbar and subsequent raising of the jacket temperature to 170° C. 1265 parts by weight of 4-methylbenzonitrile are obtained with a purity of over 98% (HPLC), and also 37 parts by weight of a mixed fraction essentially consisting of 4-methylbenzonitrile and 4-methylbenzaldehyde.

後処理

  1. stirringstirred at this temperature for 21/2 hours
  2. temperatureIt is subsequently heated at 125° C. at a pressure of 80 mbar
  3. waitheld for a further 20 minutes, during which
  4. customa total of about 480 parts by weight of water are removed by distillation
  5. distillationThe distillation of the nitrile
  6. temperaturesubsequent raising of the jacket temperature to 170° C

出典と根拠

ORDレコード
ord-758814a6aeba44c18816e41aa51dd992
出典データセット
uspto-grants-1997_04
特許番号
US05618965

関連ノート

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