関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | N-[3-(4-Piperidinomethyl-2-pyridyloxy)propyl]-2-(2-hydroxyethylthio)acetamide | HCID 19962907 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | N-[3-(4-Piperidinomethyl-2-pyridyloxy)propyl]-2-(2-acetoxyethylthio)acetamide | HCID 19962905 | 75% |
反応手順
0.49 g of N-[3-(4-piperidinomethyl-2-pyridyloxy)propyl]-2-(2-hydroxyethylthio)acetamide [prepared as described in step (b) above] was added to a mixture of 0.48 ml of acetic anhydride and 0.43 ml of pyridine, and the resulting mixture was warmed at 60° C. for 2 hours. At the end of this time, the reaction mixture was poured into ice-water and a saturated aqueous solution of sodium hydrogencarbonate was added to it. The resulting aqueous mixture was extracted with ethyl acetate. The extract was concentrated by evaporation under reduced pressure, and the concentrate was purified by column chromatography through silica gel, using a 1:9 by volume mixture of methanol and ethyl acetate as the eluent, to give 0.41 g (yield 75%) of the title compound as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05616579 |
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| 出典データセット | uspto-grants-1997_04 |
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| ORD ID | ord-528e689e82c741fab85128b6781164cd |
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| 出典メモ | uspto-grants-1997_04 |
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