関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-(2-Oxopropoxy)benzonitrile | HCID 309603 | — |
| 反応物 | Ammonium Acetate | HCID 517165 | — |
| 反応物 | Sodium cyanoborohydride | HCID 5003444 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-(4-Cyanophenoxy)-1-methylethylamine | HCID 18972799 | 27.8% |
反応手順
293 g of ammonium acetate and 16.7 g of sodium cyanoborohydride were added to a solution containing 66.5 g of 4-cyanophenoxyacetone dissolved in 1500 mL of methanol, and the resultant mixture was stirred for 30 hours at room temperature. The reaction mixture was then concentrated under reduced pressure, and acidified with concentrated hydrochloric acid. 500 mL of diethyl ether and 300 mL of water were then added thereto. Subsequently, the resultant water layer was made basic with a 5% aqueous solution of sodium hydroxide, the solution was extracted with 1000 mL of diethyl ether, and then washed with water. The organic layer was then dried over anhydrous sodium sulfate, and the diethyl ether was removed under reduced pressure. The obtained residue was distilled under reduced pressure to yield 13.0 g of the desired product (19%). Boiling point: 132° C./0.26 mmHg.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05723469 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-a811a98a5e964e1b95e931e2733e70ca |
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| 出典メモ | uspto-grants-1998_03 |
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