関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Thiazole, 2-chloro-5-(2-chloroethyl)-4-methyl- | HCID 207964 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Clomethiazole | HCID 10783 | 91% |
反応手順
To a solution of 63 g (0.32 moles) of 2-chloro-4-methyl-5-(2-chloroethyl)-thiazole in 630 cm3 of a 96% ethanol 9 g of a wet palladium on charcoal catalyst (palladium content: 8%) are added. The mixture is hydrogenated at atmospheric pressure. The termination of the reaction is indicated by the cease of the hydrogen consumption. After filtering off the catalyst the solution is evaporated, the residue is dissolved in water and the solution is neutralized with sodium hydrogen carbonate (pH 7). The separated oil is shaken out with chloroform. The residue after the evaporation of the chloroform solution is distilled under reduced pressure. 47 g (91%) of 4-methyl-5-(2-chloroethyl)-thiazole are obtained. Its boiling point is 105° C. at a pressure of 0.93 KPa, nD20 =1.5430. Its active agent content is 98.8%, determined by gas chromatography.
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-4a5508125f1d433e834989e53f13de22 |
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| 出典メモ | uspto-grants-1997_07 |
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