Chloroacetic Acid → 2-(2-Acetyl-4-fluorophenoxy)acetic acid

HRID 22735

반응식

HRID 22735 반응식
Cl[CH2:2][C:3]([OH:5])=[O:4].[CH3:6][C:7]([C:9]1[CH:14]=[C:13]([F:15])[CH:12]=[CH:11][C:10]=1[OH:16])=[O:8].[OH-].[Na+]>O>[C:7]([C:9]1[CH:14]=[C:13]([F:15])[CH:12]=[CH:11][C:10]=1[O:16][CH2:2][C:3]([OH:5])=[O:4])(=[O:8])[CH3:6]

참가 물질

5

반응물 3

HCID 300Chloroacetic AcidHCID 14798Sodium HydroxideHCID 959922-Acetyl-4-fluorophenol

생성물 1

HCID 116585522-(2-Acetyl-4-fluorophenoxy)acetic acid수율 61.2%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Chloroacetic acid (99.3 mmol, 9.4 g) was added to a suspension of 5-fluoro-2-hydroxy acetophenone (33.1 mmol, 5.1 g) in water (60 mL) containing sodium hydroxide (165.4 mmol, 6.6 g) and the reaction mixture was refluxed for 3.5 hours. The reaction mixture was cooled to room temperature, poured into a separatory funnel and the oily liquid at the bottom of the funnel was discarded. The aqueous top layer was collected, cooled to 0° C. and acidified with conc. HCl. The white precipitate was collected, and air died. The dry solid was crystallized from toluene to obtain (2-acetyl-4-fluoro-phenoxy)-acetic acid, (57%, 4.3 g).

후처리

  1. temperaturethe reaction mixture was refluxed for 3.5 hours
  2. additionpoured into a separatory funnel
  3. customThe aqueous top layer was collected
  4. temperaturecooled to 0° C.
  5. customThe white precipitate was collected
  6. customThe dry solid was crystallized from toluene

출처 및 근거

ORD 기록
ord-13a18026d45547aba987540ce67c27c7
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06849629B2

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