関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N,N'-Dimethylethylenediamine | HCID 8070 | — |
| 反応物 | Sodium Cyanide | HCID 8929 | — |
| 反応物 | Benzene, 2-bromo-1,4-dimethyl- | HCID 11121 | — |
| 反応物 | Ammonium Hydroxide | HCID 14923 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2,5-Dimethylbenzonitrile | HCID 83688 | — |
反応手順
An oven dried screw cap test tube was charged with NaCN (93 mg, 1.898 mmol), dried KI (52 mg, 0.313 mmol, 20 mol %) and CuI (30 mg, 0.158 mmol, 10 mol %), evacuated and backfilled with argon three times. 2-Bromo-1,4-dimethylbenzene (215 μL, 1.557 mmol), N,N′-dimethylethylenediamine (165 μL, 1.549 mmol) and anhydrous toluene (1 mL) were added under argon. The tube was sealed and the reaction mixture was stirred magnetically at 110° C. for 24 h. The resulting yellow suspension was cooled to room temperature, 2 mL of ethyl acetate, 1 mL of ammonium hydroxide (30%) and 1 mL of water were added. The mixture was stirred at 25° C. for 10 min, then the organic layer was washed with 1 mL of water and dried over MgSO4. The GC analysis showed consumption of the majority of the starting material, and formation of the title compound (as confirmed by GC-MS).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06888032B2 |
|---|
| 出典データセット | uspto-grants-2005_05 |
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| ORD ID | ord-9d54b481f12c4a0ea6714bbb3aa7e5a1 |
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| 出典メモ | uspto-grants-2005_05 |
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