関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 1-(4-(2-Phenylethyl)phenyl)ethan-1-one | HCID 69918 | — |
| 反応物 | Ammonium formate | HCID 2723923 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | alpha-Methyl-p-phenethylbenzylamine hydrochloride | HCID 13012107 | 73% |
反応手順
A mixture of 87.5 g (0.39 mole) of 4'-phenethylacetophenone, M.P. 67°-70° C., prepared according to R. E. Lutz et al., J. Org. Chem. 12, 617 (1947), and 98.5 g (1.56 mole) of ammonium formate is slowly heated to 150° C. with stirring. After the initial foaming has subsided the temperature of the heating bath is raised to 185°-190° C. for a period of 4 hours. Upon cooling, the mixture is treated with several portions of water. To the residue is added 75 ml of concentrated HCl. The mixture is refluxed for 2 hours and is allowed to cool. The resulting solid is collected, washed with several portions of benzene and is recrystallized from isopropanol containing about 5% of water to yield 74.0 g (73% yield) of the desired product, M.P. 212°-214° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04055561 |
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| 出典データセット | uspto-grants-1977_10 |
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| ORD ID | ord-4037f449b0584a0ba4a4169e7dfdb160 |
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| 出典メモ | uspto-grants-1977_10 |
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