関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Sulfate | HCID 24436 | — |
| 反応物 | Hydroxylamine sulfate | HCID 24846 | — |
| 反応物 | 4-(Methylthio)benzaldehyde | HCID 76985 | — |
| 生成物 | 4-(Methylthio)benzonitrile | HCID 590960 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05618965 |
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| 出典データセット | uspto-grants-1997_04 |
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| ORD ID | ord-5afa9ca9f74646d994bb235e63558a20 |
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| 出典メモ | uspto-grants-1997_04 |
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