Sodium Sulfate → 4-(Methylthio)benzonitrile

HRID 53404

反応式

HRID 53404 の反応式
S([O-])([O-])(=O)=O.[Na+].[Na+].[CH3:8][S:9][C:10]1[CH:17]=[CH:16][C:13]([CH:14]=O)=[CH:12][CH:11]=1.S([O-])([O-])(=O)=O.O[NH3+:24].O[NH3+]>>[CH3:8][S:9][C:10]1[CH:17]=[CH:16][C:13]([C:14]#[N:24])=[CH:12][CH:11]=1

参加物

4

反応物 3

HCID 24436Sodium SulfateHCID 24846Hydroxylamine sulfateHCID 769854-(Methylthio)benzaldehyde

生成物 1

HCID 5909604-(Methylthio)benzonitrile

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 4000 parts by weight of anhydrous sodium sulfate, 950 parts by weight of 4-(methylthio)benzaldehyde and 538.4 parts by weight of hydroxylammonium sulfate. Following evacuation to 25 mbar, the mixture is heated to 80° C. and stirred at this temperature for 3 hours. It is subsequently heated at 130° C. and held for 30 minutes at the same pressure. A total of about 240 parts by weight of water are removed by distillation altogether. The distillation of the nitrile is initiated and controlled by reduction of the pressure to 5 mbar and subsequent raising of the jacket temperature to 150° C. 708 parts by weight of 4-(methylthio)benzonitrile are obtained with a purity of over 98% (TLC), and also 18 parts by weight of a mixed fraction essentially consisting of 4-(methylthio)benzonitrile and 4-(methylthio)benzaldehyde. The collected 4-(methylthio)benzonitrile has a melting point of 61°-63° C.

後処理

  1. stirringstirred at this temperature for 3 hours
  2. temperatureIt is subsequently heated at 130° C.
  3. customA total of about 240 parts by weight of water are removed by distillation altogether
  4. distillationThe distillation of the nitrile
  5. temperaturesubsequent raising of the jacket temperature to 150° C

出典と根拠

ORDレコード
ord-5afa9ca9f74646d994bb235e63558a20
出典データセット
uspto-grants-1997_04
特許番号
US05618965

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