Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 3-Ethyl-1-(3-nitrophenyl)pyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Sulfurous acid, diethyl ester | HCID 12197 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 1-(m-nitrophenyl)pyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione | HCID 12760301 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 3-Ethyl-1-(3-nitrophenyl)pyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione | HCID 12764178 | 87.8% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US03984415 |
| 출처 데이터셋 | uspto-grants-1976_10 |
| ORD ID | ord-e3bf5f87350d4fe59f8c16d9f847409a |
| 출처 메모 | uspto-grants-1976_10 |