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Methyl iodide → Michler's ethylene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | 4,4'-Bis(dimethylamino)benzophenone | HCID 7031 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 反応物 | HCID 178418373 | HCID 178418373 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | Michler's ethylene | HCID 81995 | 65% |
反応手順
After adding 100 ml of benzene to a diethyl ether solution of methylmagnesium iodide prepared from 1.7 g of magnesium, 9.9 g of methyl iodide, and 100 ml of diethyl ether, 16.6 of 4,4'-bis-dimethylaminobenzophenone was gradually added thereto. After stirring at room temperature for 10 hours, the reaction mixture was decomposed by a saturated aqueous ammonium chloride solution, followed by stirring as it was for 2 hours. After separating and water-washing an organic layer, the solvent was distilled off, and the residue was recrystallized from ethanol to obtain 10.7 g of 1,1-bis(4'-dimethylaminophenyl)ethylene. The melting point was 121° to 122° C., and the theoretical yield was 65%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04751163 |
| 出典データセット | uspto-grants-1988_06 |
| ORD ID | ord-750d9f98b9574c88853959119e9817a8 |
| 出典メモ | uspto-grants-1988_06 |