Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Trifluoroacetic acid → Ethyl 4-(2-oxo-1,4-dihydropyrido[3,4-d]pyrimidin-3(2H)-yl)piperidine-1-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Trifluoroacetic acid | HCID 6422 | — |
| 반응물 | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| 반응물 | Ethyl 4-[({3-[(tert-butoxycarbonyl)amino]pyridin-4-yl}methyl)amino]piperidine-1-carboxylate | HCID 22293284 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Ethyl 4-(2-oxo-1,4-dihydropyrido[3,4-d]pyrimidin-3(2H)-yl)piperidine-1-carboxylate | HCID 22293189 | 39.7% |
반응 단계
Trifluoroacetic acid (1.43 g) was added to a solution of the material from Step A (0.47 g, 1.24 mmol) in dichloromethane (10 mL). After stirring overnight, the reaction was concentrated. This material was dissolved in acetonitrile (5 mL) and carbonyldiimidazole (0.62 g, 3.73 mmol) was added at room temperature. After 2 d, the acetonitrile was evaporated in vacuo, the residue partitioned between 1N NaOH and dichloromethane, and the organic phase dried over magnesium sulfate. The crude product was purified by chromatography (silica gel, 1 to 20% methanol in methylene chloride gradient elution), which gave the title compound (0.15 g). MS 305.2.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07745427B2 |
| 출처 데이터셋 | uspto-grants-2010_06 |
| ORD ID | ord-403bae1824544b6e9f503a53bca66f4c |
| 출처 메모 | uspto-grants-2010_06 |