関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Cyanide | HCID 9032 | — |
| 反応物 | 2-Methyl-2-phenylpropanal | HCID 283879 | — |
| 反応物 | Methylamine hydrochloride | HCID 6364545 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Methyl-2-(methylamino)-3-phenylbutanenitrile | HCID 11708193 | 95% |
反応手順
To a solution of potassium cyanide (103 g, 1.56 mol) and methylamine hydrochloride (106 g, 1.56 mol) in water (1000 mL) is added a solution of 2-methyl-2-phenylpropanal (222 g, 1.50 mol) in methanol (1000 mL) over a period of 30 minutes. An ice-water bath is used occasionally to maintain the reaction temperature between 20-25° C. The mixture is stirred at room temperature for 25 hours. Water (2000 mL) is then added and the reaction mixture is extracted with CH2Cl2 (3×800 mL). The combined organic extracts are washed with brine (500 mL) and dried over Na2SO4. The organic extracts are filtered and concentrated to give 3-methyl-2-(methylamino)-3-phenylbutanenitrile as an oil (274 g, 95% yield, 76.6% by HPLC area, NMR (>95%)). Evidence of decomposition on the HPLC/GC column is noted.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06951955B2 |
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| 出典データセット | uspto-grants-2005_10 |
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| ORD ID | ord-229183f5043d4bfca086d132b31a2fc5 |
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| 出典メモ | uspto-grants-2005_10 |
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