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海萝胶 → 1,4-二氢-2,6-二甲基-4-(3-硝基苯基)吡啶-3,5-二甲酸单甲酯
参与物
| 角色 | 名称 | HCID | 投料 |
|---|---|---|---|
| 反应物 | 海萝胶 | HCID 313 | — |
| 反应物 | 二氯甲烷 | HCID 6344 | — |
| 反应物 | 二甲基对苯二胺二盐酸 | HCID 14798 | — |
| 反应物 | 乐卡地平杂质 | HCID 10916009 | — |
| 溶剂 | 丙酮 | HCID 180 | — |
| 产物 | 1,4-二氢-2,6-二甲基-4-(3-硝基苯基)吡啶-3,5-二甲酸单甲酯 | HCID 173322 | — |
反应步骤
Next, a solution of NaOH (41.3 mL of 35% NaOH in 375 mL H2O) was slowly added to a solution of 2,6-dimethyl-3-carbomethoxy-4-(3-nitrophenyl)-5-(2-cyano)ethoxycarbonyl-1,4-dihydropyridine (80 g, 0.21 mol) in acetone (240 mL). Then, CH2Cl2 (500 mL) was added and 12N HCl (41.3 mL) slowly introduced. The resulting precipitate was filtered and recrystallized from dimethylformamide/H2O (175 mL DMF, 72 mL H2O) to yield 2,6-dimethyl-3-carbomethoxy-4-(3-nitrophenyl)-5-carboxy-1,4-dihydropyridine (mp=242° C.).
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 专利号 | US04761420 |
| 来源数据集 | uspto-grants-1988_08 |
| ORD ID | ord-edbf78708faf4c909cf5147bfc5e8c4b |
| 来源说明 | uspto-grants-1988_08 |