関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1,2-Dibromoethane | HCID 7839 | — |
| 反応物 | 3-Tolunitrile | HCID 12104 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 4-chloro-N-methylpiperidine | HCID 79342 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | (3-Methylphenyl) (1-methyl-4-piperidinyl)methanone | HCID 12852040 | — |
反応手順
To 5 parts of magnesium are added 2.18 parts of 1,2-dibromoethane and a small amount of iodine to initiate the reaction. Then there is added dropwise a solution of 28 parts of 4-chloro-1-methylpiperidine in 180 parts of tetrahydrofuran while the mixture is heated to 70° C. After cooling, there is added dropwise a solution of 14 parts of 3-methylbenzonitrile in 90 parts of tetrahydrofuran. Upon completion, stirring is continued for 1 hour at reflux temperature. The reaction mixture is cooled and poured onto a solution of 75 parts of ammonium chloride in water. The product is extracted with 2,2'-oxybispropane. The extract is washed with water, dried, filtered and evaporated, yielding 35 parts of (3-methylphenyl) (1-methyl-4-piperidinyl)methanone as an oily residue.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04342870 |
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| 出典データセット | uspto-grants-1982_08 |
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| ORD ID | ord-7766b44aae14420995ee55d945992721 |
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| 出典メモ | uspto-grants-1982_08 |
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