Sodium Hydroxide → 2-(2-Aminophenoxy)benzoic acid

HRID 1077977ノート

反応式

HRID 1077977 の反応式
[NH2:1][C:2]1[CH:18]=[CH:17][CH:16]=[CH:15][C:3]=1[O:4][C:5]1[CH:14]=[CH:13][CH:12]=[CH:11][C:6]=1[C:7]([O:9]C)=[O:8].[OH-].[Na+]>CO.O>[NH2:1][C:2]1[CH:18]=[CH:17][CH:16]=[CH:15][C:3]=1[O:4][C:5]1[CH:14]=[CH:13][CH:12]=[CH:11][C:6]=1[C:7]([OH:9])=[O:8]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 16080835HCID 16080835、化合物

生成物 1

HCID 214610602-(2-Aminophenoxy)benzoic acid

試薬・触媒・溶媒 1

HCID 22242641Methanol--water (1/1)溶媒

実験手順

A mixture of Methyl 2-(2-aminophenoxy)benzoate (9.2 g, 0.038 mol) and sodium hydroxide (3.2 g, 0.08 mol) in 1:1 methanol/water (200 mL) was stirred under argon at room temperature for 3 h. The methanol was evaporated, the aqueous residue was acidified with dilute HCl, extracted with ethyl acetate, dried over anhydrous MgSO4, filtered, and evaporated to give the crude product which was purified by flash chromatography (silica gel, ethyl acetate/hexane/formic acid), and then recrystallized from ethyl acetate/hexane to give the title compound as a white crystalline solid; mp 150°-151° C.

後処理

  1. customThe methanol was evaporated
  2. extractionextracted with ethyl acetate
  3. dry with materialdried over anhydrous MgSO4
  4. filtrationfiltered
  5. customevaporated
  6. customto give the crude product which
  7. customwas purified by flash chromatography (silica gel, ethyl acetate/hexane/formic acid)
  8. customrecrystallized from ethyl acetate/hexane

出典と根拠

ORDレコード
ord-925c8c3f2ddd42c691e12134fefa79fc
出典データセット
uspto-grants-1996_08
特許番号
US05545669

反応ノート

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