Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Diethyl 2-(ethoxymethylidene)-3-oxobutanedioate → Diethyl 5-ethylpyridine-2,3-dicarboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Diethyl 2-(ethoxymethylidene)-3-oxobutanedioate | HCID 40590 | — |
| 반응물 | 1-Morpholinobutene | HCID 580977 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Diethyl 5-ethylpyridine-2,3-dicarboxylate | HCID 10857926 | 57% |
반응 단계
Diethyl ethoxymethyleneoxalacetate (3.17 g, 0.013 mol) is added to a solution of 1-morpholinobutene (1.84 g, 0.013 mol) dissolved in CH2Cl2 (40 mL) at 0°. The solution is concentrated in vacuo, and ammonium acetate (50 g), ammonium hydroxide (10 mL), tetrahydrofuran (20 mL) and 95% ethanol (20 mL) are added. The solution is heated to reflux for 30 minutes, then held at 3° for 72 hours. The reaction solution is then partitioned between water and ethyl acetate. The organic layer is dried over sodium sulfate and concentrated in vacuo to give the product (1.85 g, 0.0074 mol, 57%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05622913 |
| 출처 데이터셋 | uspto-grants-1997_04 |
| ORD ID | ord-c97b5599ce8c4fe7bd8e9e468c4dd726 |
| 출처 메모 | uspto-grants-1997_04 |