Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetic Acid → 2-[2-(Pyrrolidin-1-yl)ethylthio]methyl-3,5-dicarboethoxy-4-(m-nitrophenyl)-6-methyl-1,4-dihydropyridine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | 1-(2-Chloroethyl)pyrrolidine hydrochloride | HCID 81668 | — |
| 반응물 | Sodium ethoxide | HCID 2723922 | — |
| 반응물 | 2-Mercaptomethyl-3,5-dicarboetoxy-4-(m-nitrophenyl)-6-methyl-1,4-dihydropyridine | HCID 11675833 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | 2-[2-(Pyrrolidin-1-yl)ethylthio]methyl-3,5-dicarboethoxy-4-(m-nitrophenyl)-6-methyl-1,4-dihydropyridine | HCID 19831186 | 41.8% |
반응 단계
A solution of 2-(pyrrolidin-1-yl)-1-chloroethane hydrochloride (2.8 g), 2-mercaptomethyl-3,5-dicarboethoxy-4-(m-nitrophenyl) -6-methyl-1,4-dihydropyridine (5.4 g) and sodium ethoxide (2 g) in ethanol (70 ml) is heated to the reflux temperature for 6 hours, then it is neutralized with AcOH and evaporated under reduced pressure. The residue, after the usual work-up, is purified by column-chromatography (SiO2 ; 210 g; eluent AcOH/MeOH 99/1) to give 2.8 g of 2-[2-(pyrrolidin-1-yl)ethylthio]methyl-3,5-dicarboethoxy-4-(m-nitrophenyl) -6-methyl-1,4-dihydropyridine, as an oil, that upon treatment with fumaric acid gives the corresponding salt, m.p. 192°-194° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04999362 |
| 출처 데이터셋 | uspto-grants-1991_03 |
| ORD ID | ord-8228bc68d1484fdaa0c278a4d67104d6 |
| 출처 메모 | uspto-grants-1991_03 |