関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,5-Dibromopentane | HCID 8100 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Cyanoacetate | HCID 1551036 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Ethyl 1-cyanocyclohexane-1-carboxylate | HCID 10997650 | 57% |
反応手順
To a solution of cyanoacetate (1 eq) in DMF at 0° C. was slowly added cesium carbonate (2.5 eq), followed by the slow addition of 1,5-dibromopentane. This mixture was allowed to stir for 30 minutes at 0° C. and at room temperature for two hours. The crude reaction mixture was diluted with ethyl acetate and washed three times with water, dried with anhydrous sodium sulfate, filtered, and concentrated. The compound was clean enough to continue without purification. 57% yield. 1H NMR (300 MHz, CDCl3) δ 4.25 (q, 2H), 2.12-1.68 (m, 10H), 1.31 (t, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08173689B2 |
|---|
| 出典データセット | uspto-grants-2012_05 |
|---|
| ORD ID | ord-250348398b5f488c9c00aef0bbb2c6c4 |
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| 出典メモ | uspto-grants-2012_05 |
|---|
