関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Chlorobenzyl chloride | HCID 11906 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 4,5,6,7-Tetrahydrothieno(3,2-c)pyridine | HCID 3085076 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Ticlopidine Hydrochloride | HCID 65335 | — |
反応手順
26.1 g of 4,5,6,7-tetrahydrothieno[3,2-c]pyridine, 80 ml of ethanol and 19 g of sodium bicarbonate are charged into a 250-ml three-necked round bottom flask fitted with a thermometer, a condenser and a mechanical stirrer. 30.2 g of o-chlorobenzyl chloride are then added and the mixture is heated to about 75°-80° C. during 1 hour. The reaction mixture is evaporated down and the residue is taken up with 200 ml of isopropyl ether. The 5-(2-chlorobenzyl)-4,5,6,7-tetrahydrothieno[3,2-c]pyridine obtained is then added to 100 ml of ethanol. After adding 20 ml of concentrated hydrochloric acid to the ethanolic solution, heating to reflux and cooling the mixture, 46.6 g of 5-(2-chlorobenzyl)-4,5,6,7-tetrahydrothieno[3,2-c]pyridine hydrochloride, which crystallises, are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05132435 |
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| 出典データセット | uspto-grants-1992_07 |
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| ORD ID | ord-d123dc5eb5e04e5fb8b7094929ab233c |
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| 出典メモ | uspto-grants-1992_07 |
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