Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → diethyl 3-(m-chlorophenyl)-4-methyl-2-oxo-2H-pyrano[2,3-b]pyridine-6,7-dicarboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Ammonium Hydroxide | HCID 14923 | — |
| 반응물 | 3-Chlorophenylacetic acid | HCID 15879 | — |
| 반응물 | Diethyl 5-acetyl-1,6-dihydro-6-oxo-2,3-pyridinedicarboxylate | HCID 13752508 | — |
| 용매 | Acetic Anhydride | HCID 7918 | — |
| 생성물 | diethyl 3-(m-chlorophenyl)-4-methyl-2-oxo-2H-pyrano[2,3-b]pyridine-6,7-dicarboxylate | HCID 19958197 | 95.1% |
반응 단계
Diethyl 5-acetyl-1,6-dihydro-6-oxo-2,3-pyridinedicarboxylate (12.0 g, 0.043 mol), 3-chlorophenyl acetic acid (7.33 g, 0.043 mol) and triethylamine (6.52 g) are refluxed in 120 mL of acetic anhydride for three hours. The reaction mixture is cooled, poured into 120 mL of ice-cold water and made alkaline to pH 8 with an ammonium hydroxide solution. The crystalline solid is filtered and washed with water to give (17.0 g, 95%) of the product after drying. Recrystallization from ethyl acetate affords the pure product (13.29, 74% yield), melting point 170°-172° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05622913 |
| 출처 데이터셋 | uspto-grants-1997_04 |
| ORD ID | ord-300e0b1a711340a3858babc405d9b684 |
| 출처 메모 | uspto-grants-1997_04 |