関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Pyridinemethanamine | HCID 19509 | — |
| 反応物 | 6-(2,6-Dichlorophenyl)-8-methyl-2-(methylthio)pyrido[2,3-d]pyrimidin-7(8H)-one | HCID 10736701 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-aminopyrido[2,3-d]pyrimidin-7(8H)-one 34 | HCID 5327881 | 38.7% |
反応手順
A mixture of 0.165 g (0.47 mmol) of 6-(2,6-dichlorophenyl)-8-methyl-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 37, 1.08 g (10.0 mmol) of 2-(aminomethyl)pyridine and 0.5 mL of dimethylformamide was heated with stirring in a 130° C. oil bath. After 2 minutes, solution was complete. After 2 hours, the excess amine and dimethylformamide were evaporated at reduced pressure. Ether (5 mL) was added to the residue. Crystals immediately developed. Water (5 mL) was added, and the entire mixture was filtered. The cake was washed 5 mL of ether, 5 mL of water, and then dried; wt 0.164 g. Recrystallization from ethyl acetate gave 0.075 g of pure product; mp 198°-201° 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-4065ebd450dd42b9b396a7e3dbade98c |
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| 出典メモ | uspto-grants-1998_03 |
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