関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | 4,6-Dichloro-n-methylpyrimidin-2-amine | HCID 259880 | — |
| 反応物 | 5-Chloro-2-ethoxyphenylboronic acid | HCID 3700836 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | 2,3-Butanediol | HCID 262 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | [4-Chloro-6-(5-chloro-2-ethoxy-phenyl)-pyrimidin-2-yl]-methyl-amine | HCID 86004334 | 91.5% |
反応手順
To an argon saturated solution of N-(4,6-dichloro-pyrimidin-2-yl)-methyl-amine (200 mg, 1.1 mmol), 5-chloro-2-ethoxy-phenylboronic acid (248 mg, 1.21 mmol) and palladium acetate (38 mg, 0.16 mmol) in dimethyl ethylene glycol (20 ml) was added a solution of sodium carbonate (240 mg, 2.2 mmol) in water (5 ml) followed by triphenylphosphine (66 mg, 0.33 mmol). After stirring at 70° C. under an argon atmosphere for 60 hours, the mixture was filtered through a pad of celite under suction and the filtrate was dried over magnesium sulfate. Evaporation of the solvent under reduced pressure provided [4-chloro-6-(5-chloro-2-ethoxy-phenyl)-pyrimidin-2-yl]-methyl-amine (300 mg, 90% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07419984B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-092e9e7a5b8a433aa456fb1bf7873c0d |
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| 出典メモ | uspto-grants-2008_09 |
|---|
