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p-Toluenesulfonic acid monohydrate → HCID 18615089、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 反応物 | Ethyl 4-acetylbenzoate | HCID 600911 | — |
| 溶媒 | Ethylene Glycol | HCID 174 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | HCID 18615089 | HCID 18615089 | — |
反応手順
ethyl 4-acetyl-benzoate (9.61 g, a product of the firm Wako Pure Chemical Ind.) was dissolved in toluene (200 ml) under an argon atmosphere whereto ethylene glycol (20 ml) and p-toluenesulfonic acid hydrate (200 mg) were added, whereupon the mixture was refluxed with heating for 24 hours while dehydrating on a Dean-Stark apparatus. After cooling down to room temerature, the toluene layer was washed with water (100 ml×twice) and with saturated aqueous sodium chloride solution (100 ml) succeedingly, followed by drying and concentrating to dryness under reduced pressure, whereby the above-identified compound was obtained (12.76 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06172099B2 |
| 出典データセット | uspto-grants-2001_01 |
| ORD ID | ord-4162c50c57c448d4880a91b9ace26986 |
| 出典メモ | uspto-grants-2001_01 |