関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | Furfural | HCID 7362 | — |
| 反応物 | 2,3-Butanedithiol | HCID 548353 | — |
| 溶媒 | Cyclohexane | HCID 8078 | — |
| 生成物 | 2-(4,5-Dimethyl-1,3-dithiolan-2-yl)furan | HCID 20398676 | — |
反応手順
Into a 100 ml reaction flask equipped with magnetic stirring bar, thermometer and reflux condenser and hot plate with magnetic stirring apparatus is placed 0.5 grams para-toluenesulfonic acid, 5 ml cyclohexane and 6.1 grams (0.05 moles) of 2,3-butanedithiol. Over a period of 35 minutes, 4.8 grams (0.05 moles) of 2-furaldehyde is added to the reaction mass with stirring. The reaction mass is then heated to reflux and refluxed for a period of 7.5 hours with stirring while removing water to reaction. After the refluxing period, the reaction mass is cooled to room temperature and transferred to a separatory funnel. The reaction mass is then washed with one 50 ml portion of saturated sodium chloride soution and dried over anhydrous sodium sulfate and filtered. The resulting filtrate is distilled using a Microvigreux column yielding the following fractions:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04514429 |
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| 出典データセット | uspto-grants-1985_04 |
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| ORD ID | ord-dbaec3954a164b598dde9ac66f44baf9 |
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| 出典メモ | uspto-grants-1985_04 |
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