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Sodium Hydroxide → 2-Bromo-[1,2,4]triazolo[1,5-a]pyridine-7-carboxylic acid

HRID 874351
ノート
印刷プレビュー

反応式

HRID 874351 の反応式
[OH-].[Na+].[Br:3][C:4]1[N:16]=[C:7]2[CH:8]=[C:9]([C:12]([O:14]C)=[O:13])[CH:10]=[CH:11][N:6]2[N:5]=1>CO>[Br:3][C:4]1[N:16]=[C:7]2[CH:8]=[C:9]([C:12]([OH:14])=[O:13])[CH:10]=[CH:11][N:6]2[N:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 90383439Methyl 2-bromo-[1,2,4]triazolo[1,5-a]pyridine-7-carboxylate

生成物 1

HCID 838249652-Bromo-[1,2,4]triazolo[1,5-a]pyridine-7-carboxylic acid収率 95.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A 1 N sodium hydroxide aqueous solution (150 ml) was added to a methanol (150 ml) suspension of the methyl 2-bromo-[1,2,4]triazolo[1,5-a]pyridine-7-carboxylate (10 g) obtained in (Example 3.15) <Step 2>, and the obtained mixture was then stirred for 30 minutes. Thereafter, about half of the solvent was distilled away under reduced pressure, and the residue was then adjusted to pH 4 by addition of 3 N hydrochloric acid (50 ml). The precipitated solid was collected by filtration, and was then successively washed with water (50 ml) and methyl tert-butyl ether (20 ml). The obtained solid was, subjected to azeotropy with toluene to obtain the title compound (9.0 g) in the form of a white solid.

後処理

  1. customobtained in (Example 3.15) <Step 2>
  2. distillationThereafter, about half of the solvent was distilled away under reduced pressure
  3. additionthe residue was then adjusted to pH 4 by addition of 3 N hydrochloric acid (50 ml)
  4. filtrationThe precipitated solid was collected by filtration
  5. washwas then successively washed with water (50 ml) and methyl tert-butyl ether (20 ml)

出典と根拠

ORDレコード
ord-609c08ecc4cd451782e3037b7bb5b9e3
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08980888B2

反応ノート

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