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

HRID 22735

反応式

HRID 22735 の反応式
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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-13a18026d45547aba987540ce67c27c7
出典データセット
uspto-grants-2005_02
特許番号
US06849629B2

関連ノート

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