Nitric Acid → 6-Bromo-3-nitroimidazo[1,2-a]pyridine

HRID 614849ノート

反応式

HRID 614849 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([CH:8]=[CH:9][N:10]=2)[CH:7]=1.S(=O)(=O)(O)O.[N+:16]([O-])([OH:18])=[O:17].[OH-].[K+]>>[N+:16]([C:8]1[N:6]2[CH:7]=[C:2]([Br:1])[CH:3]=[CH:4][C:5]2=[N:10][CH:9]=1)([O-:18])=[O:17]

参加物

5

反応物 4

HCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 14797Potassium HydroxideHCID 27955476-Bromoimidazo[1,2-a]pyridine

生成物 1

HCID 288758886-Bromo-3-nitroimidazo[1,2-a]pyridine

実験手順

A solution of 24 gms. (0.122 mole) of 6-bromoimidazo [1,2-a] pyridine in 80 ml. of concentrated sulfuric acid is treated dropwise with 24 ml. of concentrated nitric acid while maintaining a temperature of 15° C. with external cooling. When the addition is complete, the reaction mixture is stirred at room temperature for 1/2 hour and poured onto 450 gm. of ice. The pH of the mixture is adjusted to pH 4 with aqueous potassium hydroxide and the resultant solids are collected by filtration. The filter cake is washed with water and dried. Recrystallization from methylene chloride-hexane yields pure 3-nitro 6-bromoimidazo [1,2-a] pyridine m.p. 160°-161° C.

後処理

  1. additionWhen the addition
  2. additionpoured onto 450 gm
  3. filtrationthe resultant solids are collected by filtration
  4. washThe filter cake is washed with water
  5. customdried
  6. customRecrystallization from methylene chloride-hexane

出典と根拠

ORDレコード
ord-06caeeee2e464de998da9acc60a5625a
出典データセット
uspto-grants-1979_03
特許番号
US04146642

反応ノート

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