関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | 4-Nitrobenzyl bromide | HCID 66011 | — |
| 反応物 | 2-(2-Amino-6-chloro-pyrimidin-4-yl)-4-bromo-phenol | HCID 136080012 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | HCID 178508398 | HCID 178508398 | — |
反応手順
A stirred suspension of 2-(2-amino-6-chloro-pyrimidin-4-yl)-4-bromo-phenol (0.151 g, 0.50 mmol), 1-bromomethyl-4-nitro-benzene (0.218 g, 1.0 mmol), and cesium carbonate (0.325 g, 1.0 mmol) in acetonitrile (10 ml) was stirred at 80° C. for 2 hours. Filtration and concentration of the filtrate provided a crude product which was dissolved in ethyl acetate (10 ml) and stirred while a 4 M solution of hydrogen chloride in dioxane (0.50 ml, 2.0 mmol) was added. Filtration provided 6-[5-bromo-2-(4-nitro-benzyloxy)-phenyl]-6-chloro-pyrimidin-2-ylamine as hydrochloride salt (0.23 g, 96% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07419984B2 |
|---|
| 出典データセット | uspto-grants-2008_09 |
|---|
| ORD ID | ord-bdd88fb03a0342c4a0570f3bdc97a1a4 |
|---|
| 出典メモ | uspto-grants-2008_09 |
|---|
