Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Isopropyl3-aminocrotonate → Isopropyl 2-methoxyethyl 4-(2-fluorophenyl)-1,4-dihydro-2,6-dimethylpyridine-3,5-dicarboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Isopropyl3-aminocrotonate | HCID 3271821 | — |
| 반응물 | Toluene ethylacetate | HCID 21584019 | — |
| 반응물 | 2-Methoxyethyl 2-acetyl-3-(2-fluorophenyl)-2-propenoate | HCID 59957778 | — |
| 용매 | Isopropanol | HCID 3776 | — |
| 생성물 | Isopropyl 2-methoxyethyl 4-(2-fluorophenyl)-1,4-dihydro-2,6-dimethylpyridine-3,5-dicarboxylate | HCID 15295381 | 48% |
반응 단계
4.0 g (about 15 mmol) of the compound from Example I are heated to reflux overnight in 100 ml of isopropanol with 2.2 g (15 mmol) of isopropyl 3-amino-2-butenoate. After thin-layer chromatographic checking (SiO2, toluene/ethyl acetate 5:1) shows complete conversion, the reaction mixture is concentrated, the residue is taken up with toluene, the solution is concentrated again and the residue is then purified by filtration on silica gel (eluent: toluene/ethyl acetate 100:1-5:1). A crystallizing yellow oil is obtained, which is recrystallized from methanol at about −15° C. 2.8 g (48%) of the target compound are obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06630494B2 |
| 출처 데이터셋 | uspto-grants-2003_10 |
| ORD ID | ord-10106c774ecb41e2a1b1683c35aac6d4 |
| 출처 메모 | uspto-grants-2003_10 |