関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Iodoethane | HCID 6340 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | HCID 178418283 | HCID 178418283 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-amino-6-(2,6-dichlorophenyl)-8-ethyl-7H,8H-pyrido[2,3-d]pyrimidin-7-one | HCID 5328625 | 55.4% |
反応手順
To a suspension of NaH (60% in mineral oil, 27 mg) in 5 mL of dimethylformamide was added 2-amino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]pyrimidin-7(8H)-one (172 mg, 0.56 mmol) from Example 11. The mixture was heated at 50° C. for 1 hour resulting in a clear solution. Ethyl iodide (60 μL, 0.75 mmol) was added, and the solution was stirred at 50° C. for 3.5 hours, cooled to room temperature, and poured into 30 mL of ice water. The resulting precipitate was removed by filtration and partitioned between ethyl acetate and water. The organic layer was separated and dried over MgSO4, filtered, and concentrated in vacuo. Flash chromatography, eluting with ethyl acetate, provided 104 mg (55%) of 2-amino-6-(2,6-dichlorophenyl)-8-ethyl-pyrido[2,3-d]pyrimidin-7(8H)-one; mp 207°-209° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05733914 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-dc089cf7000c4b12a70b5ffd130e6b36 |
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| 出典メモ | uspto-grants-1998_03 |
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