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Water → 3-Ethyl-1-(3-nitrophenyl)pyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sulfurous acid, diethyl ester | HCID 12197 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1-(m-nitrophenyl)pyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione | HCID 12760301 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-Ethyl-1-(3-nitrophenyl)pyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione | HCID 12764178 | 87.8% |
反応手順
2.8 g of 1-(m-nitrophenyl)pyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione was dissolved in 30 ml of dry dimethylformamide. To the solution was added 0.6 g of about 50 % sodium hydride, and stirring was performed for 30 minutes. To the mixture was further added 3.5 g of diethylsulfite and the whole was reacted for 2 hours at room temperature. After the reaction was finished, the solvent was distilled off from the mixture under reduced pressure. To the residue thus obtained was added water to precipitate a crude product. This product was recrystallized from methanol to yield 2.7 g of 1-(m-nitrophenyl)-3-ethylpyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione as pale yellow prisms, melting at 210°-211°C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US03984415 |
| 出典データセット | uspto-grants-1976_10 |
| ORD ID | ord-e3bf5f87350d4fe59f8c16d9f847409a |
| 出典メモ | uspto-grants-1976_10 |