関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Butyl iodide | HCID 10962 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-Amino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]pyrimidin-7-ol | HCID 10494915 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-amino-8-butyl-6-(2,6-dichlorophenyl)-8H-pyrido[2,3-d]pyrimidin-7-one | HCID 5328627 | 64% |
反応手順
To a suspension of NaH (60% in mineral oil, 34 mg) in 6 mL of dimethylformamide was added 2-amino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]pyrimidin-7(8H)-one (202 mg, 0.66 mmol). The mixture was heated to 50° C., resulting in a clear solution. 1-Iodobutane (105 μL, 0.92 mmol) was added, and the solution was stirred at 50° C. for 30 minutes, then cooled to room temperature and poured onto 40 mL of ice water. The resulting precipitate was removed by filtration and washed with water. The residue was dried and purified by flash chromatography, eluting with a gradient of 1:1 hexane:ethyl acetate to all ethyl acetate to provide 152 mg (64%) of 2-amino-8-butyl-6-(2,6-dichlorophenyl)-8H-pyrido[2,3-d]pyrimidin-7-one; mp 202°-205° 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-01a5e0a168094896bccae2b3b8ee6758 |
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| 出典メモ | uspto-grants-1998_03 |
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