Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triphenyl phosphite → Methyl 4-methyl-2-oxo-1,2,3,4-tetrahydropyrido[2,3-b]pyrazine-7-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triphenyl phosphite | HCID 7540 | — |
| 반응물 | Methyl 6-((2-methoxy-2-oxoethyl)(methyl)amino)-5-nitronicotinate | HCID 58324470 | — |
| 반응물 | HCID 178418361 | HCID 178418361 | — |
| 촉매 | Platinum | HCID 23939 | — |
| 촉매 | Ammonium metavanadate | HCID 516859 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Methyl 4-methyl-2-oxo-1,2,3,4-tetrahydropyrido[2,3-b]pyrazine-7-carboxylate | HCID 58324455 | 68.8% |
반응 단계
Methyl 6-((2-methoxy-2-oxoethyl)(methyl)amino)-5-nitronicotinate (2.7 g, 9.53 mmol) was dissolved in dichloromethane (10 mL). To the yellow solution was added ammonium metavanadate (30.0 mg, 0.256 mmol), triphenyl phosphite (aprox 30 ul, 0.097 mmol), and Pt/C (300 mg, 5% w/w). The reaction mixture was pressurized with hydrogen gas (110 psi) and stirred at room temperature for 16 h. The reaction was then depressurized and diluted with dichloromethane (100 mL) which was then refluxed for 30 min. The hot solution was filtered through a pad of celite and washed with hot dichloromethane (3×20 mL). The filtrate was concentrated in vacuo to yield the title compound (1.45 g, 68%) as a white solid. [M+H] calc'd for C10H11N3O3, 222; found, 222.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08822470B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-aeca5177558b4cc7ad06a462e8e935d4 |
| 출처 메모 | uspto-grants-2014_09 |