関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Methoxyphenol | HCID 9007 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | N2-(6-chloropyrimidin-4-yl)pyridine-2,6-diamine | HCID 57708264 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | N2-(6-(3-methoxylphenoxy)pyrimidin-4-yl)pyridine-2,6-diamine | HCID 57708231 | 40.7% |
反応手順
To a solution of N2-(6-chloropyrimidin-4-yl)pyridine-2,6-diamine (200 mg, 0.90 mmol) in dry DMF (2 mL) was added 3-methoxyphenol (112 mg, 0.90 mmol) and anhydrous K2CO3 (186 mg, 1.353 mmol). The reaction mixture was heated at 100° C. for 16 h under N2 atmosphere. It was then cooled and DMF removed under reduced pressure to give a yellowish gummy residue that was taken in EtOAc (10 mL). It was washed with water (5 mL), brine (5 mL), dried over Na2SO4 and then concentrated under reduced pressure to give a crude product. This was further purified by column chromatography (SiO2, 60-120, hexane/EtOAc, 5/5) to give N2-(6-(3-methoxylphenoxy)pyrimidin-4-yl)pyridine-2,6-diamine (110 mg, 40.7%) as a pale yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08748606B2 |
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| 出典データセット | uspto-grants-2014_06 |
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| ORD ID | ord-085fc37d00d94cbab6701e9d978d0e48 |
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| 出典メモ | uspto-grants-2014_06 |
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