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2-Pyrrolidone → 1-(1,4-Dioxaspiro[4.5]decan-8-yl)pyrrolidin-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Pyrrolidone | HCID 12025 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1,4-Dioxaspiro(4.5)decan-8-yl methanesulfonate | HCID 14966741 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-(1,4-Dioxaspiro[4.5]decan-8-yl)pyrrolidin-2-one | HCID 10900293 | 11.5% |
反応手順
Pyrrolidin-2-one (720 mg, 8.46 mmol) in DMF (5 mL) was treated with NaH (203 mg, 8.46 mmol) at room temperature. The mixture allowed to stir for 30 min. 1,4-dioxaspiro[4.5]decan-8-yl methanesulfonate (500 mg, 2.12 mmol) from above step A, in DMF (3 mL) was added to the mixture and stirred at 130° C. for 3 h. The mixture was cooled to room temperature, quenched with NH4Cl, and extracted into EtOAc. Washed the EtOAc layer with saturated NaCl, dried over Na2SO4 and evaporated. Purified by silica prep TLC to give 55 mg (11.5%) of 1-(1,4-dioxaspiro[4.5]decan-8-yl)pyrrolidin-2-one.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08518969B2 |
| 出典データセット | uspto-grants-2013_08 |
| ORD ID | ord-2ce2d8c96c8d4a18932ee09386df8c9e |
| 出典メモ | uspto-grants-2013_08 |