化工社化工社 化学情報印刷レポート · 研究参考用
Iodoethane → 2,2-Diethylmalononitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Iodoethane | HCID 6340 | — |
| 反応物 | Malononitrile | HCID 8010 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 触媒 | Tetrabutylammonium Bromide | HCID 74236 | — |
| 生成物 | 2,2-Diethylmalononitrile | HCID 2777231 | — |
反応手順
Malononitrile (15.2 g) was mixed with TBAB (3.0 g, 4 mol %) and ethyl iodide (36.8 mL, 2 equiv.). After stirring for 30 minutes at room temperature, the mixture was cooled in an ice bath, KOtBu (51.6 g, 2 equiv.) was added portionwise, the ice bath was removed, and the mixture was stirred for 30 minutes at room temperature. Extraction with DCM/H2O, drying over Na2SO4 and evaporation under reduced pressure gave 40 grams of crude material, which was purified by flash chromatography eluting with DCM. This yielded 20.4 grams of an orange oil which solidified upon standing. 1H NMR (400 MHz, CDCl3) δ 1.29 (t, J=7.5 Hz, 6H), 2.00 (q, J=7.5 Hz, 4H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07728018B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-70c666ce7b4a4ede94971688eaf95325 |
| 出典メモ | uspto-grants-2010_06 |