Water → 4-Chloro-2-fluoro-1-(2,2,2-trifluoroethoxy)benzene

HRID 1098508

反応式

HRID 1098508 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[C:4]([F:9])[CH:3]=1.[F-].[K+].[F:12][C:13]([F:17])([F:16])[CH2:14]I.O>CO>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:14][C:13]([F:17])([F:16])[F:12])=[C:4]([F:9])[CH:3]=1

参加物

6

反応物 4

HCID 962WaterHCID 677091,1,1-Trifluoro-2-iodoethaneHCID 1819754-Chloro-2-fluorophenolHCID 522689Potassium Fluoride

生成物 1

HCID 595067484-Chloro-2-fluoro-1-(2,2,2-trifluoroethoxy)benzene

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
50 °C

実験手順

To 4-Chloro-2-fluoro-phenol (521, 5.0 g, 0.034 mol) in methanol (50.0 mL) was added potassium fluoride (2.2 g, 0.038 mol). The solvent was removed. The resulting salt was added to N,N-dimethylformaldehyde (25 mL), followed by adding 1,1,1-trifluoro-2-iodo-ethane (8.60 g, 40.9 mmol). The reaction was stirred at 50° C. overnight. The reaction was poured into water and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated and purified by silica gel column chromatography eluting with 20% ethyl acetate in hexane to give colorless oil (522, 2.0 g, 26%).

後処理

  1. customThe solvent was removed
  2. additionThe resulting salt was added to N,N-dimethylformaldehyde (25 mL)
  3. extractionextracted with ethyl acetate
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated
  7. custompurified by silica gel column chromatography
  8. washeluting with 20% ethyl acetate in hexane
  9. customto give colorless oil (522, 2.0 g, 26%)

出典と根拠

ORDレコード
ord-6f27ff4e3db344cea051d96aa76bea9a
出典データセット
uspto-grants-2012_03
特許番号
US08143271B2

関連ノート

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