Hydrochloric Acid → 3-Amino-4,5-diethoxycarbonyl-2-phenyl-6-sulfopyridine

HRID 37511ノート

反応式

HRID 37511 の反応式
C(OC([C:6]1([N+:27]([O-])=O)[C:11]([C:12]([O:14][CH2:15][CH3:16])=[O:13])=[CH:10][C:9]([S:17]([OH:20])(=[O:19])=[O:18])=[N:8][CH:7]1[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)=O)C.Cl>C(O)C>[NH2:27][C:6]1[C:7]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)=[N:8][C:9]([S:17]([OH:20])(=[O:18])=[O:19])=[C:10]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[C:11]=1[C:12]([O:14][CH2:15][CH3:16])=[O:13]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 199355933,4-Diethoxycarbonyl-3-nitro-2-phenyl-6-sulfopyridine

生成物 1

HCID 152897053-Amino-4,5-diethoxycarbonyl-2-phenyl-6-sulfopyridine収率 152.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
60 °C

実験手順

A mixture of 0.34 g of 3,4-diethoxycarbonyl-3-nitro-2-phenyl-6-sulfopyridine, 0.41 g of reduced iron and 7 ml of ethanol was heated to 60° C., and then 0.5 ml of conc. hydrochloric acid was added. The mixture was heated under reflux for 20 minutes. After the reaction mixture was concentrated to dryness, the residue was subjected to silica gel column chromatography (eluent:chloroform/methanol 5:1), to give 0.24 g of the title compound as pale yellow crystals.

後処理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 20 minutes
  3. concentrationAfter the reaction mixture was concentrated to dryness

出典と根拠

ORDレコード
ord-a0ae2db61f414b338b9f80a607d7bf72
出典データセット
uspto-grants-1995_05
特許番号
US05420275

反応ノート

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