참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | HCID 178418283 | HCID 178418283 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-amino-6-(2,6-dichlorophenyl)-8-methyl-7H,8H-pyrido[2,3-d]pyrimidin-7-one | HCID 5327864 | 49.1% |
반응 단계
To a mixture of 2-amino-6-(2,6-dichlorophenyl)pyrido[2,3-d]pyrimidin-7-ol (3.7 g) from Example 11 in dimethylformamide was added NaH (50% suspension in mineral oil, 0.64 g). The resulting slurry was heated at 65° C. for 0.5 hour until a solution formed. It was then cooled to 50° C. and a solution of methyl iodide (2.0 g) in dimethylformamide (10 mL) was added dropwise to the reaction. The reaction mixture was warmed and kept between 60° C.-80° C. for 3 hours. Upon cooling to room temperature, the reaction mixture was poured into ice water. The insoluble white product was filtered, washed with water, and recrystallized from ethanol using charcoal to give 1.9 g of 2-amino-6-(2,6-dichlorophenyl)-8-methyl-pyrido[2,3 -d]pyrimidin-7(8H)-one, mp 235°-237° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05620981 |
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| 출처 데이터셋 | uspto-grants-1997_04 |
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| ORD ID | ord-5b94812b2cb04f379c12b9c616eef059 |
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| 출처 메모 | uspto-grants-1997_04 |
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