Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Nitrogen → 2,6-dimethyl-3-(6-morpholinopyridin-3-yl)pyrimidin-4(3H)-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Nitrogen | HCID 947 | — |
| 반응물 | 6-(Morpholino)pyridin-3-amine | HCID 104059 | — |
| 반응물 | 2-Butenoic acid, 3-(acetylamino)-, methyl ester, (2Z)- | HCID 5705360 | — |
| 반응물 | Trimethylaluminum | HCID 16682925 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2,6-dimethyl-3-(6-morpholinopyridin-3-yl)pyrimidin-4(3H)-one | HCID 72948757 | 39% |
반응 단계
To a solution of 6-morpholinopyridin-3-amine (1.79 g, 10 mmol) in CH2Cl2 (100 mL) was added trimethylaluminium (40 mL, 40 mmol, 1 M in heptane) carefully under N2. The mixture was stirred at rt for 30 min, followed by the addition of a solution of methyl 3-acetaminocrotonate (1.89 g, 12 mmol) in CH2Cl2 (5 mL). The reaction was stirred at rt for 6 h, then quenched with saturated NH4Cl aqueous solution (100 mL). The organic phase was dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by recrystallized from EtOAc to give the title compound as a pale yellow solid (1.11 g, 39%). The compound was characterized by the following spectroscopic data:
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09434695B2 |
| 출처 데이터셋 | uspto-grants-2016_09 |
| ORD ID | ord-69d5c9da52714651bccbd451dd45290a |
| 출처 메모 | uspto-grants-2016_09 |