関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methylamine | HCID 6329 | — |
| 反応物 | Methyl 1-benzyl-5-oxopyrrolidine-3-carboxylate | HCID 98909 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 1-benzyl-N-methyl-5-oxopyrrolidine-3-carboxamide | HCID 13491794 | 88.4% |
反応手順
A mixture of 100 g (0.43 mole) of methyl 5-oxo-1-(phenylmethyl)-3-pyrrolidinecarboxylate [J. Org. Chem., 26, 1519 (1961)], 500 ml methanol and 100 g (3.2 mole) of methylamine was heated at 100° C. in a pressure reactor for 16 hours. The reaction mixture was cooled and the ammonia and methanol were removed under reduced pressure. The residue was taken up in dichloromethane and washed with 3×100 ml 1N sodium hydroxide. The organic layer was dried over magnesium sulfate and the solvent removed at reduced pressure to give 88.3 g of N-methyl-5-oxo-1-(phenylmethyl)-3-pyrrolidinecarboxamide as a white solid, mp 82.5°-83.0° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04604401 |
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| 出典データセット | uspto-grants-1986_08 |
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| ORD ID | ord-4b7e98998c2043f1ab9442150b84b674 |
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| 出典メモ | uspto-grants-1986_08 |
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