関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | (2S, 4S)-1-(t-butoxycarbonyl)-2-carbamoyl-4-(4-methoxybenzylthio)pyrrolidine | HCID 14880265 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | (2S, 4S)-2-Carbamoyl-4-(4-methoxybenzylthio)-pyrrolidine | HCID 14880267 | 97.5% |
反応手順
1.92 g of (2S, 4S)-1-(t-butoxycarbonyl)-2-carbamoyl-4-(4-methoxybenzylthio)pyrrolidine [prepared as described in step (4) above] was dissolved in 25 ml of ethyl acetate, and 26.2 ml of a 4N dioxane solution of hydrogen chloride were added to the solution, whilst ice-cooling. The mixture was then stirred at 0° to 5° C. for 2 hours and at room temperature for 30 minutes. At the end of this time, it was poured into a saturated aqueous solution of sodium bicarbonate, to make it weakly basic, and was extracted with ethyl acetate. The extract was washed with an aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate. The solvent was then removed by distillation under reduced pressure, to give 1.36 g of the title compound as a powder, melting at 120°-121° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05104867 |
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| 出典データセット | uspto-grants-1992_04 |
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| ORD ID | ord-ba4569551baf46c690fc02dcd6230f62 |
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| 出典メモ | uspto-grants-1992_04 |
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