Nitric Acid → HCID 18983889、化合物

HRID 1440467ノート

反応式

HRID 1440467 の反応式
[CH2:1]([O:3][C:4]([C:6]1[N:7]=[C:8]2[C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[CH:12][CH:11]=[CH:10][N:9]2[CH:19]=1)=[O:5])[CH3:2].[N+:20]([O-])([OH:22])=[O:21].[OH-].[Na+]>S(=O)(=O)(O)O>[CH2:1]([O:3][C:4]([C:6]1[N:7]=[C:8]2[C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[CH:12][CH:11]=[CH:10][N:9]2[C:19]=1[N+:20]([O-:22])=[O:21])=[O:5])[CH3:2]

参加物

5

反応物 3

HCID 944Nitric AcidHCID 14798Sodium HydroxideHCID 189838522,8-Diethyl imidazo[1,2-a]pyridine-2,8-dicarboxylate

生成物 1

HCID 18983889HCID 18983889、化合物収率 53.8%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

Ethyl 2-ethoxycarbonylimidazo[1,2-a]pyridine-8-carboxylate (3.8 g, 14.5 m mol) was dissolved in conc. sulfuric acid (10 ml), and to the solution was slowly added 70% nitric acid (1.5 ml) at 10° C. The mixture was stirred at room temperature for 30 minutes, poured into ice water and adjusted to pH 7 by adding 20% sodium hydroxide. The precipitated crystals were filtered to obtain ethyl 2-ethoxycarbonyl-3-nitro-imidazo[1,2-a]pyridine-8-carboxylate (2.4 g, yield 53.8%) as crystals of m.p. 139°-140° C. A solution of the crystals in conc. hydrochloric acid (35 ml) was refluxed for 1.5 hours and cooled to room temperature. The precipitated crystals were collected by filtration and dried to give the object compound (1.2 g, yield 74.3%) of m.p.>300° C.

後処理

  1. customat 10° C
  2. filtrationThe precipitated crystals were filtered

出典と根拠

ORDレコード
ord-d8d857799f544678a0ac714e1dabf544
出典データセット
uspto-grants-1996_03
特許番号
US05498774

反応ノート

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