関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3,5-Dichloropentan-2-one | HCID 94032 | — |
| 反応物 | Potassium thiocyanate | HCID 516872 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 3-Thiocyanato-5-chloro-2-pentanone | HCID 10877693 | 93% |
反応手順
77.8 g (0.5 moles) of 3,5-dichloro-2-pentanone [prepared according to Acta Chim. Hung. 3, 157 (1953)] are added to the solution of 49.9 g (0.513 moles) of potassium rhodanide in 500 ml of acetone. The solution is boiled under stirring for 4 hours. The reaction mixture is cooled to room temperature and the precipitated potassium chloride is filtered off and washed with acetone. The filtrate is evaporated, the residue is dissolved in benzene and the benzene solution is washed 3 times with water. After drying with sodium sulphate, the benzene is distilled off. 62.2 g (93%) of 3-thiocyanato-5-chloro-2-pentanone are obtained in the form of a red oil. After distilling at a lower pressure a faint yellow oil is obtained, its boiling point is 112° C. at a pressure of 26.6 Pa, nD20 =1.5110. According to infrared spectrum it does not contain any isothiocyanate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05648498 |
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| 出典データセット | uspto-grants-1997_07 |
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| ORD ID | ord-582e2a8ee0294ad7ae44b9b9cccae218 |
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| 出典メモ | uspto-grants-1997_07 |
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