Hydrochloric Acid → 2,6-Dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylic acid monomethyl ester

HRID 34412

反応式

HRID 34412 の反応式
[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]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 6344DichloromethaneHCID 14798Sodium HydroxideHCID 109160093,5-Pyridinedicarboxylic acid, 1,4-dihydro-2,6-dimethyl-4-(3-nitrophenyl)-, 3-(2-cyanoethyl) 5-methyl ester

生成物 1

HCID 1733222,6-Dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylic acid monomethyl ester

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

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.).

後処理

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

出典と根拠

ORDレコード
ord-edbf78708faf4c909cf5147bfc5e8c4b
出典データセット
uspto-grants-1988_08
特許番号
US04761420

関連ノート

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