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Dimethyl Sulfoxide → N-[(6-methylpyridin-2-yl)methyl]-N-pyridin-2-ylpyridin-2-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethyl Sulfoxide | HCID 679 | — |
| 反応物 | 2,2'-Dipyridylamine | HCID 14547 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 2-(Bromomethyl)-6-methylpyridine | HCID 12543733 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | N-[(6-methylpyridin-2-yl)methyl]-N-pyridin-2-ylpyridin-2-amine | HCID 66628202 | — |
反応手順
To a flask were added 0.6 g pulverized potassium hydroxide and 15 ml dimethylsulfoxide. After adding 1.4 g of 2,2′-dipyridylamine, the mixture was stirred under nitrogen for 45 minutes, when 1.5 g 6-methyl-2-(bromomethyl)pyridine was added. After stirring for 1 hour, 35 ml of water was added and the product was extracted with 60 ml of 50% ethyl acetate, 50% hexane. The organic layer was washed with 30 ml water and the solvent was removed. The residue was purified by silica gel chromatography using 48% ethyl acetate, 48% hexane, and 4% methanol resulting in 2.0 g of an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08431045B2 |
| 出典データセット | uspto-grants-2013_04 |
| ORD ID | ord-faa27bf9f09e4feeb7427d393ce37fcc |
| 出典メモ | uspto-grants-2013_04 |