関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | 3-Bromo-5-methylaniline | HCID 3018526 | — |
| 反応物 | 2-Chloro-4-methylpyrimidine | HCID 11629607 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | N-(3-bromo-5-methylphenyl)-4-methylpyrimidin-2-amine | HCID 67249356 | 100% |
反応手順
Acetic acid (0.234 mL, 4.08 mmol) was added to 2-chloro-4-methylpyrimidine (0.5 g, 3.89 mmol) and 3-bromo-5-methylaniline (1.096 g, 3.89 mmol) suspended in dioxane (7.78 mL). The reaction was heated to 120° C. overnight. Then, the reaction was cooled to room temperature and was directly purified by column chromatography on silica gel eluting with ethyl acetate/hexanes to give N-(3-bromo-5-methylphenyl)-4-methylpyrimidin-2-amine (1.08 g, 3.89 mmol, quant.) as a white solid. MS ESI: [M+H]+ m/z 278.0 and 280.0.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08551984B2 |
|---|
| 出典データセット | uspto-grants-2013_10 |
|---|
| ORD ID | ord-70deb626fe5c4457b6daf6a44871850d |
|---|
| 出典メモ | uspto-grants-2013_10 |
|---|
