3-Nitrobenzaldehyde → 2-Amino-6-dimethylamino-4-(3'-nitrophenyl)-4,5-dihydropyridine-3,5-dicarboxylic acid diethyl ester

HRID 1415293ノート

反応式

HRID 1415293 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([CH:9]=[CH:10][CH:11]=1)[CH:7]=O)([O-:3])=[O:2].[CH2:12]([O:14][C:15](=[O:22])[CH:16]=[C:17]([N:19]([CH3:21])[CH3:20])[NH2:18])[CH3:13]>C(O)C>[CH2:12]([O:14][C:15]([C:16]1[CH:7]([C:6]2[CH:9]=[CH:10][CH:11]=[C:4]([N+:1]([O-:3])=[O:2])[CH:5]=2)[CH:16]([C:15]([O:14][CH2:12][CH3:13])=[O:22])[C:17]([N:19]([CH3:20])[CH3:21])=[N:18][C:17]=1[NH2:18])=[O:22])[CH3:13]

参加物

4

反応物 2

HCID 74493-NitrobenzaldehydeHCID 867334643-Amino-3-dimethylaminoacrylic acid ethyl ester

生成物 1

HCID 124486892-Amino-6-dimethylamino-4-(3'-nitrophenyl)-4,5-dihydropyridine-3,5-dicarboxylic acid diethyl ester

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

After boiling a solution of 7.5 g of 3-nitrobenzaldehyde and 15.8 g of N,N-dimethyl-3,3-diaminoacrylic acid ethyl ester in 150 ml of ethanol for 4 hours, the solution was concentrated in vacuo. On triturating the resulting oil with ether, filtering off the crystals which separated out and crystallizing these from isopropanol, the yellow-orange colored crystals of 2-amino-6-dimethylamino-4-(3'-nitrophenyl)-4,5-dihydropyridine-3,5-dicarboxylic acid diethyl ester, of melting point 149° C, were obtained. Yield, 61% of theory.

後処理

  1. customfor 4 hours
  2. concentrationthe solution was concentrated in vacuo
  3. customOn triturating the resulting oil with ether
  4. filtrationfiltering off the crystals which
  5. customseparated out
  6. customcrystallizing these from isopropanol

出典と根拠

ORDレコード
ord-45286f4ad3ae4df6a81171266e5ac153
出典データセット
uspto-grants-1977_01
特許番号
US04004014

反応ノート

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