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Potassium Iodide → 6-Acetylamino-1-[N-(4-cyclohexylbutan-1-yl)-N-methylaminomethyl]indan
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Cyclohexylbutan-1-ol mesylate | HCID 10376753 | — |
| 反応物 | 6-Acetylamino-1-(N-methylaminomethyl)indan | HCID 21834210 | — |
| 溶媒 | Methyl Isobutyl Ketone | HCID 7909 | — |
| 生成物 | 6-Acetylamino-1-[N-(4-cyclohexylbutan-1-yl)-N-methylaminomethyl]indan | HCID 21834236 | — |
反応手順
A mixture of 6-Acetylamino-1-(N-methylaminomethyl)indan (1.5 g), 4-cyclohexylbutan-1-ol mesylate (2.5 g), potassium carbonate (1.4 g), and a crystal of potassium iodide in MIBK (80 ml) were refluxed for 5 h. After cooling inorganic salts were filtered off and the solvent evaporated in vacuo. The remaining oil was subjected to column chromatography on SiO2 (eluted with ethyl acetate: heptane: triethylamine 80:20:4). The free base of the title compound was isolated as an oil. The sesquioxalate of 13a crystallized from acetone. Yield 1.6 g Mp: 145-155° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05972964 |
| 出典データセット | uspto-grants-1999_10 |
| ORD ID | ord-3b420eefaa4f4ba4ba22be7391d00899 |
| 出典メモ | uspto-grants-1999_10 |