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HRID 406951作成日:2026年10月27日
p-Toluenesulfonic acid → (2R,4aR,10bR)-6-(2,6-Dimethoxy-pyridin-3-yl)-9-ethoxy-8-methoxy-1,2,3,4,4a,10b-hexahydro-phenanthridin-2-ol tosylate
https://huagongshe.com/reaction/406951
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
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| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | (2R,4aR,10bR)-6-(2,6-Dimethoxy-pyridin-3-yl)-9-ethoxy-8-methoxy-1,2,3,4,4a,10b-hexahydro-phenanthridin-2-ol | HCID 11258441 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | (2R,4aR,10bR)-6-(2,6-Dimethoxy-pyridin-3-yl)-9-ethoxy-8-methoxy-1,2,3,4,4a,10b-hexahydro-phenanthridin-2-ol tosylate | HCID 87240041 | 97.1% |
反応手順
(2R,4aR,10bR)-6-(2,6-Dimethoxy-pyridin-3-yl)-9-eth oxy-8-methoxy-1,2,3,4,4a,10b-hexahydro-phenanthridin-2-ol (1.5 g; 3.6 mmol) is dissolved in 9 ml of 2-propanol. The solution is heated up to 60° C. 723 mg (3.8 mmol) of p-toluenesulfonic acid are added. The solution is cooled down to room temperature and stirred over night. From a part of the solution seed crystals are produced and added to the remaining solution. The crystals are filtered off and dried to obtain 1.98 g (94%) of the title compound (m.p.: 218° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08754218B2 |
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| 出典データセット | uspto-grants-2014_06 |
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| ORD ID | ord-56b430f4f3fe446f87361241da96b70a |
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| 出典メモ | uspto-grants-2014_06 |
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