関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Chloride | HCID 5234 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Methyl (2S,4R)-4-methylsulfonyloxy-1-methyl-2-pyrrolidinecarboxylate | HCID 12082503 | — |
| 反応物 | Potassium ethanethioate | HCID 23670855 | — |
| 溶媒 | Water ethanol | HCID 19096565 | — |
| 生成物 | methyl (2S,4S)-4-acetylthio-1-methyl-2-pyrrolidinecarboxylate | HCID 12082502 | 97.4% |
反応手順
Potassium thioacetate (677 mg) was added to a solution of methyl (2S,4R)-4-methylsulfonyloxy-1-methyl-2-pyrrolidinecarboxylate (609 mg) obtained from Reference example 4 in ethanol/water (9:1) (6 ml), and the resulting mixture was stirred at 80° C. for 3 hours, and then the mixture was allowed to stand overnight at the same temperature. Ethyl acetate (20 mL) and 10% aqueous sodium chloride solution (10 mL) were added to the reaction mixture, which was then extracted. The organic layer was separated from the aqueous layer, which was washed with water (10 mL). The solvent of the organic layer was removed by distillation under reduced pressure to give the title compound (543 mg, yield 97%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07091363B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-c3fa110c818b49349c5d166723b662c8 |
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| 出典メモ | uspto-grants-2006_08 |
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