反応 #62690

反応方程式

HCl

NaOH

2,6-dimethyl-3-carbomethoxy-4-(3-nitrophenyl)-5-(2-cyano)ethoxycarbonyl-1,4-dihydropyridine

CH2Cl2

→

2,6-dimethyl-3-carbomethoxy-4-(3-nitrophenyl)-5-carboxy-1,4-dihydropyridine

溶媒

acetone

反応条件

後処理

1. 1
   ろ過The resulting precipitate was filtered
2. 2
   その他recrystallized from dimethylformamide/H2O (175 mL DMF, 72 mL H2O)

実験手順

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.).

出典