関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethyl Malonate | HCID 7761 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 2-Cyclohexen-1-one | HCID 13594 | — |
| 反応物 | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1,3-Diethyl 2-(3-oxocyclohexyl)propanedioate | HCID 317049 | 104% |
反応手順
A solution of cyclohex-2-enone (3.05 mL, 30 mmol) and diethyl malonate (4.58 mL, 30.0 mmol) in THF (30 mL) was treated with 1,8-diazabicyclo[5.4.0]undec-7-ene (4.52 mL, 30.0 mmol) and heated at 50° C. for 16 h. The cooled mixture was poured into EtOAc and washed sequentially with 1M aqueous HCl and brine. The combined aqueous layers were extracted with EtOAc, and the combined organic phases were dried and concentrated to give diethyl 2-(3-oxocyclohexyl)malonate as an oil (8.0 g), used without further purification. Mass spectrum m/z 257 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09334290B2 |
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| 出典データセット | uspto-grants-2016_05 |
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| ORD ID | ord-a2ea0672ee5743b9ad4173f2ddb94550 |
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| 出典メモ | uspto-grants-2016_05 |
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