関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Furanmethanethiol | HCID 7363 | — |
| 反応物 | 4-Chlorobutyronitrile | HCID 12336 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-((Furan-2-ylmethyl)thio)butanenitrile | HCID 21273287 | 94.1% |
反応手順
A solution of sodium hydroxide (12.7 g) in water (50 ml) and ethanol (50 ml) was added dropwise over 30 minutes to a solution of furanylmethyl mercaptan (34.25 g) and 4-chlorobutyronitrile (31.58 g) in ethanol (150 ml) under nitrogen at 10° C. (ice-bath). The temperature rose slightly (to 18° C.) and the solution went cloudy. It was stirred at room temperature for 6.5 hours and allowed to stand for 20 hours. Ethanol was removed by evaporation at reduced pressure. The residue was dissolved in water (100 ml) and the solution was extracted with chloroform . The combined extracts were washed with water, dried (MgSO4) and chloroform evaporated at reduced pressure. The residual light-brown liquid was vacuum-distilled to give 4-(2-furanylmethylthio)butyronitrile (51.16 g), b.p.0.05 mm 112°-5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04808589 |
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| 出典データセット | uspto-grants-1989_02 |
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| ORD ID | ord-8f1bcfeab7f34c849acc3a624dd88f59 |
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| 出典メモ | uspto-grants-1989_02 |
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