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Malononitrile → 2,2-Bis-(2,2,2-trifluoro-ethyl)-malononitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Malononitrile | HCID 8010 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1,1,1-Trifluoro-3-iodopropane | HCID 156165 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2,2-Bis-(2,2,2-trifluoro-ethyl)-malononitrile | HCID 86625410 | 16.4% |
反応手順
Malononitril (20.15 mmol) and 1-iodo-3,3,3-trifluoropropane (42.65 mmol) were dissolved in 30 ml dry THF, and the mixture was cooled with an ice/salt bath. 1.61 g NaH (40.3 mmol) was added portionwise, keeping the temperature below 5° C. The reaction mixture was stirred at room temperature for 2 hours and evaporated under reduced pressure. The crude material was purified by flash chromatography eluting with DCM, yielding 0.76 grams of an oil. 1H NMR (400 MHz, CDCl3) δ 2.62-2.49 (m, 4H), 2.31-2.24 (m, 4H)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08722887B2 |
| 出典データセット | uspto-grants-2014_05 |
| ORD ID | ord-cbc0d984f3a944c9a7df439d4f780def |
| 出典メモ | uspto-grants-2014_05 |