関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | HCID 178433533 | HCID 178433533 | — |
| 溶媒 | Chlorobenzene | HCID 7964 | — |
| 生成物 | Thiazole, 2-chloro-5-(2-chloroethyl)-4-methyl- | HCID 207964 | 74% |
反応手順
A suspension of 177.6 g (1 mole) of 2-hydroxy-4-methyl-5-(2-chloroethyl)-thiazole in 530 cm3 of anhydrous chlorobezene is heated to 100° C. under stirring. 306.6 g (2 moles) of phosphoryl chloride are flown into the solution in 30 minutes, then it is stirred at a temperature of 125°-130° C. until the formation of hydrogen chloride ceases (about 2 hours). The reaction mixture is cooled to 20° C., then it is poured onto 1.5 kg of ice. The phases are separated, the aqueous phase is extracted twice with 200 cm3 of chlorobenzene each. The combined phases containing the chlorobenzene are washed acid-free with water and then with a 5% sodium hydrogen carbonate solution and then evaporated under reduced pressure. The brown residue is fractionated in vacuo. 145 g (74%) of 2-chloro-4-methyl-5-(2-chloroethyl)thiazole are obtained. The boiling point is 102° C. at a pressure of 53.2 Pa, n20D =5512, n30D =1,5468.
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-79fe91567f404754a10a89ce0d59848e |
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| 出典メモ | uspto-grants-1997_07 |
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