Water → 4-Amino-2-fluorobenzoic acid

HRID 401759

反応式

HRID 401759 の反応式
[NH2:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#N)=[C:4]([F:10])[CH:3]=1.[OH-:11].[K+].[OH2:13]>>[NH2:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]([OH:13])=[O:11])=[C:4]([F:10])[CH:3]=1

参加物

4

反応物 3

HCID 962WaterHCID 14797Potassium HydroxideHCID 27834134-Amino-2-fluorobenzonitrile

生成物 1

HCID 3026804-Amino-2-fluorobenzoic acid収率 84%

実験手順

A mixture of 4-amino-2-fluorobenzonitrile (25 g, 0.183 mmol) and potassium hydroxide (125 g, 2.23 mol) in water (350 ml) and industrial methylated spirit (50 ml) was heated at reflux for 48 hours. The solvent was evaporated in vacuo and the residue diluted with water and washed with DCM. The aqueous phase was acidified to pH 5.5 with concentrated HCl and the resultant precipitate collected by filtration to yield the title compound as a beige solid (23.94 g, 0.154 mol 84%).

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 48 hours
  3. customThe solvent was evaporated in vacuo
  4. additionthe residue diluted with water
  5. washwashed with DCM
  6. filtrationthe resultant precipitate collected by filtration

出典と根拠

ORDレコード
ord-98ee07d618d34a62834a1590fdcd4bb1
出典データセット
uspto-grants-2014_06
特許番号
US08741934B2

関連ノート

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