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Water → 2-Methyl-2-[(S)-5-oxo-1-((S)-1-phenyl-ethyl)-pyrrolidin-3-ylmethyl]-malonic Acid Dimethyl Ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Dimethyl methylmalonate | HCID 69104 | — |
| 反応物 | (S)-4-Iodomethyl-1-((S)-1-phenyl-ethyl)-pyrrolidin-2-one | HCID 10830178 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 2-Methyl-2-[(S)-5-oxo-1-((S)-1-phenyl-ethyl)-pyrrolidin-3-ylmethyl]-malonic Acid Dimethyl Ester | HCID 59094041 | 81% |
反応手順
To dimethyl methylmalonate (1.06 g, 7.29 mmol) in DMSO (7 mL) at room temperature was added NaH (291 mg of a 60% dispersion in oil). After the effervescence had ceased the lactam 85 (2 g, 7.29 mol) in DMSO (5 mL) was added. After 1 hour water was added and the aqueous solution extracted with ether. The combined organic extracts were dried (MgSO4) and concentrated. Flash chromatography (1:1 hexane/acetone) of the residue gave the product as an oil (1.7 g, 81%). MS m/z 348 (M+H, 100%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07189747B2 |
| 出典データセット | uspto-grants-2007_03 |
| ORD ID | ord-30e5fbd17ebc45b78420476ccbf0b13c |
| 出典メモ | uspto-grants-2007_03 |