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Ammonia → 4,5,6,7-Tetrahydrothieno[2,3-c]pyridin-4-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | 2,2-diethoxy-N-(thiophen-2-ylmethyl)ethanamine | HCID 2795396 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 生成物 | 4,5,6,7-Tetrahydrothieno[2,3-c]pyridin-4-ol | HCID 12337023 | 28.5% |
反応手順
2,2-Diethoxy-N-(thiophen-2-ylmethyl)ethaneamine (72.5 g) prepared in the step 2 was dissolved in 5N aqueous solution of hydrochloric acid and stirred overnight at room temperature. The reaction solution was neutralized with 10% aqueous ammonia and subjected to extraction with ethyl acetate. The organic layer was separated, washed with water and a saturated solution of sodium chloride successively, dried over anhydrous magnesium sulfate and the solvent was evaporated therefrom in vacuo. The residue was purified by silica gel column chromatography to give 14.0 g of the objective compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08217031B2 |
| 出典データセット | uspto-grants-2012_07 |
| ORD ID | ord-08eb0dac5f7d41f381ee68cbddfad073 |
| 出典メモ | uspto-grants-2012_07 |