Water → 4-Amino-2-fluorobenzoic acid

HRID 401759

반응식

HRID 401759 반응식
[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

참가 물질

4

반응물 3

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

생성물 1

HCID 3026804-Amino-2-fluorobenzoic acid수율 84%

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-98ee07d618d34a62834a1590fdcd4bb1
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08741934B2

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