Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetic Acid → Methyl 2-oxo-1-phenyl-1,2-dihydropyridine-3-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | (E)-Dimethyl 2-(3-(phenylamino)allylidene)malonate | HCID 59852887 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | Methyl 2-oxo-1-phenyl-1,2-dihydropyridine-3-carboxylate | HCID 59852857 | 92.1% |
반응 단계
To a solution of (E)-dimethyl 2-(3-(phenylamino)allylidene)malonate (130 mg, 0.50 mrnol) in methanol (8 mL) at rt was added NaH (50 mg of the 60% NaH in oil, 1.2 mmol) and the mixture was stirred at rt for 3 h. Acetic acid (0.3 mL) was added to the mixture, concentrated to a volume of 4 mL, and purificationof the reaction mixture by preparative HPLC provided the desired product (105 mg, 92%) as a yellow solid. 1H NMR (CD3OD) δ 8.30 (dd, 1H, J=7.2, 2.2 Hz), 7.87 (dd, 1H, J=6.6, 1.7 ), 7.57-7.38 (m, 5H), 6.53 (t, 1H, J=7.0 Hz), 3.84 (s, 3H); MS(ESI+) m/z 230.3 (M+H)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07566784B2 |
| 출처 데이터셋 | uspto-grants-2009_07 |
| ORD ID | ord-27163c00b8f645abae144b6820a6c023 |
| 출처 메모 | uspto-grants-2009_07 |