참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Sulfate | HCID 24436 | — |
| 반응물 | Hydroxylamine sulfate | HCID 24846 | — |
| 반응물 | 4-(Methylthio)benzaldehyde | HCID 76985 | — |
| 생성물 | 4-(Methylthio)benzonitrile | HCID 590960 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05618965 |
|---|
| 출처 데이터셋 | uspto-grants-1997_04 |
|---|
| ORD ID | ord-5afa9ca9f74646d994bb235e63558a20 |
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| 출처 메모 | uspto-grants-1997_04 |
|---|
