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Sodium Hydroxide → 3-Bromo-5-(3-pyridyl)benzoic Acid

HRID 431878
ノート
印刷プレビュー

反応式

HRID 431878 の反応式
C[O:2][C:3](=[O:17])[C:4]1[CH:9]=[C:8]([C:10]2[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=2)[CH:7]=[C:6]([Br:16])[CH:5]=1.[OH-].[Na+]>CO>[Br:16][C:6]1[CH:5]=[C:4]([CH:9]=[C:8]([C:10]2[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=2)[CH:7]=1)[C:3]([OH:17])=[O:2]
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 21942604Methyl-3-bromo-5-(3-pyridyl)benzoate

生成物 1

HCID 219425193-Bromo-5-(3-pyridyl)benzoic Acid収率 136.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

In a 100 ml round bottom flask equipped with stir bar added Methyl-3-bromo-5-(3-pyridyl)benzoate (1.16 g, 3.96 mmol), methanol (15 ml) and sodium hydroxide (5.94 ml, 5.94 mmol, 1N aqueous). Stirred the resulting mixture at 50° C. for 2 h. The reaction mixture was cooled to room temperature, concentrated in-vacuo and the residue was dissolved in methanol (20 ml). To this mixture added hydrochloric acid (1N diethyl ether) dropwise and stirred at room temperature for 10 min. The reaction mixture was concentrated in-vacuo and the residue was triturated with diethyl ether to provide the crude hydrochloride salt of title compound (1.50 g) as a white solid.

後処理

  1. customIn a 100 ml round bottom flask equipped
  2. stirringStirred the resulting mixture at 50° C. for 2 h
  3. concentrationconcentrated in-vacuo
  4. dissolutionthe residue was dissolved in methanol (20 ml)
  5. additionTo this mixture added hydrochloric acid (1N diethyl ether) dropwise
  6. stirringstirred at room temperature for 10 min
  7. concentrationThe reaction mixture was concentrated in-vacuo
  8. customthe residue was triturated with diethyl ether

出典と根拠

ORDレコード
ord-a1c08a42373644baa6b01b0f72c699f3
出典データセット
uspto-grants-2003_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06660753B2

反応ノート

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