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Water → 1,1-Dicyanocyclopentane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Malononitrile | HCID 8010 | — |
| 反応物 | 1,4-Dibromobutane | HCID 8056 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1,1-Dicyanocyclopentane | HCID 15172035 | — |
反応手順
Sodium hydride (37.8 g; 0.94 moles) was suspended in dimethylformamide (250 mL) under an atmosphere of N2. A solution of malononitrile (30 g; 0.45 moles) and 1,4-dibromobutane 99.7 g; 0.45 moles) in dimethylformamide (150 mL) was added dropwise at such a rate so as not to exceed 30° C. The mixture was stirred for overnight, poured into H2O (500 mL), and then washed with two portions of ethyl ether. The organics were combined, washed with brine, and dried over magnesium sulfate. The drying agent was removed by filtration and the filtrate was concentrated in vacuo, leaving a bilayered liquid. The lower portion was separated (28.8 g) and identified as the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05646170 |
| 出典データセット | uspto-grants-1997_07 |
| ORD ID | ord-3764906f1ab348f6bd1bcd3e514095c1 |
| 出典メモ | uspto-grants-1997_07 |