Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methanol → 4-(4-Fluorophenyl)-3-oxo-3,4-dihydropyrazine-2-carboxylic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | 4-(4-Fluorophenyl)-3-oxo-3,4-dihydropyrazine-2-carbonitrile | HCID 67347247 | — |
| 생성물 | 4-(4-Fluorophenyl)-3-oxo-3,4-dihydropyrazine-2-carboxylic acid | HCID 67349489 | — |
반응 단계
A mixture of 4-(4-fluorophenyl)-3-oxo-3,4-dihydropyrazine-2-carbonitrile (0.42 g, 1.95 mmol) and H2SO4 (4.16 mL, 78.1 mmol) was stirred at room temperature for 17 hours. Then the reaction mixture (amide intermediate) was added to MeOH (50 mL), and then the reaction was heated to 70° C. for 2.5 hours. The reaction mixture (methyl ester compound) was quenched with ice-water and treated with aq. 2N NaOH solution (for hydrolysis) at 0° C. The mixture was acidified with aq. 1N HCl, extracted with EtOAc, dried over MgSO4, and concentrated to afford 0.315 g (69% for 3-step process in one pot reaction) of the desired product which was rinsed with Et2O. 1H-NMR (400 MHz, DMSO-d6) δ 7.90 (d, 1H), 7.60 (m, 2H), 7.52 (d, 1H), 7.42 (t, 2H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08003662B2 |
| 출처 데이터셋 | uspto-grants-2011_08 |
| ORD ID | ord-e60ee085bea948ec99847ad95433e725 |
| 출처 메모 | uspto-grants-2011_08 |