関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethylene Glycol | HCID 8117 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | 2-Hexanoylthiophene | HCID 520264 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Hexylthiophene | HCID 87793 | 83% |
反応手順
In a 10 liter-five-necked flask, 300 g (1.65 mol) of 2-hexanoylthiophene, 582.1 ml of 60% hydrazine hydrate and 5 liter of diethyleneglycol were placed and reacted for 2 hours at 180° C. with distilling-off of excessive water and hydrazine hydrate. The mixture was cooled to 110° C. and 313.7 g of KOH was added thereto, followed by heating again for 2 hours of reaction at 180° C. After the reaction, the reaction mixture was poured into 10 liter of water, extracted two times with 2 liter of isopropyl ether and washed four times with 2 liter of water, followed by drying with CaCl2 and distilling-off of the solvent to obtain 285 g of a crude product. The crude product was subjected to reduced-pressure distillation in an atmosphere of nitrogen to obtain 230 g of a pure product (yield: 83%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05118441 |
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| 出典データセット | uspto-grants-1992_06 |
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| ORD ID | ord-a2fa46fbb1ef4387894e240704c77cc1 |
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| 出典メモ | uspto-grants-1992_06 |
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