関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Diethylene Glycol | HCID 8117 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 15-Hydroxy-12-ketopentadecanoic acid | HCID 9881955 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 15-Hydroxypentadecanoic acid | HCID 78360 | 85% |
反応手順
1.00 g (3.68 millimole) of 15-hydroxy-12-ketopentadecanoic acid, 0.73 g (11.0 millimole) of 85 wt.% potassium hydroxide, 0.50 g (8.5 millimole) of 85 % hydrated hydrazine and 5 ml of diethylene glycol were charged into a frask and heated under reflux over 1.5 hours. Subsequently, while evaporating the produced light boiling components such as water to the outside of the system, the internal temperature was elevated to 195 to 205° C., and the heating under reflux was continued at the same temperature range over 2 hours. After completion of the reaction, the solution was cooled, diluted by addition of 5 ml of water and added with 3 ml of 6N-HCl, followed by collection of the precipitated pail brown solid by filtration. The solid was recrystallized from benzene to obtain 0.81 g (3.14 millimole, Yield: 85 %) of a white crystl.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05023351 |
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| 出典データセット | uspto-grants-1991_06 |
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| ORD ID | ord-bc798a77a48a49ffaf13ef4043394149 |
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| 出典メモ | uspto-grants-1991_06 |
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