Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl iodide → 1-Methyl-2-oxo-1,2-dihydropyridine-3-carboxylic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Potassium Hydroxide | HCID 14797 | — |
| 반응물 | 2-Hydroxynicotinic acid | HCID 69114 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 1-Methyl-2-oxo-1,2-dihydropyridine-3-carboxylic acid | HCID 1201510 | — |
반응 단계
To 2-oxo-1H-pyridine-3-carboxylic acid (2.00 g, 14.4 mmol) in methanol (20 mL) was added a solution of KOH (1.60 g, 28.5 mmol) in water (3 mL) and the mixture was vigorously stirred until a thick suspension formed. Iodomethane (10 μL, 0.16 mmol) was added and the mixture was heated at reflux for 1.5 h. The mixture was concentrated to ⅓ volume and was acidified to pH 1 with 6N HCl. The solids were filtered off and were washed with water (3×2 mL) and acetonitrile (2×2 mL), and then dried in vacuo to give 1-methyl-2-oxo-pyridine-3-carboxylic acid as a white solid. ESI-MS m/z calc 153.0. found 154.1 (M−1)−. Retention time: 0.65 minutes (3 min run).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08598164B2 |
| 출처 데이터셋 | uspto-grants-2013_12 |
| ORD ID | ord-03398f8c8f004d69ba67d611336215a2 |
| 출처 메모 | uspto-grants-2013_12 |