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1-Methyl-4-[4-nitro-3-(propan-2-yloxy)phenyl]pyridinium iodide → 4-(1-Methylpiperidin-4-yl)-2-(propan-2-yloxy)aniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Methyl-4-[4-nitro-3-(propan-2-yloxy)phenyl]pyridinium iodide | HCID 86697964 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Platinum oxide monohydrate | HCID 86587499 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4-(1-Methylpiperidin-4-yl)-2-(propan-2-yloxy)aniline | HCID 68360001 | 96.7% |
反応手順
A solution of 10 g of 1-methyl-4-[4-nitro-3-(propan-2-yloxy)phenyl]pyridinium iodide in 280 ml of methanol is hydrogenated in an autoclave on 2.9 g of platinum oxide hydrate, at a hydrogen pressure of 15 bar and at ambient temperature for 4 h. The catalyst is removed by filtration on Clarcel and the mixture is concentrated under vacuum. The residue is taken up in 200 ml of ethyl acetate and washed with 200 ml of 1M sodium hydroxide and then with a saturated sodium chloride solution. The organic phase is dried over magnesium sulfate and concentrated under vacuum, so as to obtain 6.0 g of 4-(1-methylpiperidin-4-yl)-2-(propan-2-yloxy)aniline.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09115140B2 |
| 出典データセット | uspto-grants-2015_08 |
| ORD ID | ord-946ca97885874ef1b5b284a4e52a64f0 |
| 出典メモ | uspto-grants-2015_08 |