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

HRID 34412

反应方程式

HRID 34412 反应方程式
[OH-].[Na+].[CH3:3][C:4]1[NH:5][C:6]([CH3:30])=[C:7]([C:23]([O:25][CH2:26]CC#N)=[O:24])[CH:8]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([N+:20]([O-:22])=[O:21])[CH:15]=2)[C:9]=1[C:10]([O:12]C)=[O:11].C(Cl)Cl.Cl>CC(C)=O>[CH3:30][C:6]1[NH:5][C:4]([CH3:3])=[C:9]([C:10]([OH:12])=[O:11])[CH:8]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([N+:20]([O-:22])=[O:21])[CH:15]=2)[C:7]=1[C:23]([O:25][CH3:26])=[O:24]

参与物

6

反应物 4

HCID 313海萝胶HCID 6344二氯甲烷HCID 14798二甲基对苯二胺二盐酸HCID 10916009乐卡地平杂质

产物 1

HCID 1733221,4-二氢-2,6-二甲基-4-(3-硝基苯基)吡啶-3,5-二甲酸单甲酯

试剂、催化剂与溶剂 1

HCID 180丙酮溶剂

实验过程

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.).

后处理

  1. filtrationThe resulting precipitate was filtered
  2. customrecrystallized from dimethylformamide/H2O (175 mL DMF, 72 mL H2O)

来源与证据

ORD记录
ord-edbf78708faf4c909cf5147bfc5e8c4b
来源数据集
uspto-grants-1988_08
专利号
US04761420

关联笔记

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