Hydrochloric Acid → 2-Allyl-3,6-difluorophenol

HRID 1384071ノート

反応式

HRID 1384071 の反応式
C([O:4][C:5]1[CH:10]=[C:9]([F:11])[CH:8]=[CH:7][C:6]=1[F:12])C=C.Cl.CN(C)[C:16]1[CH:21]=CC=C[CH:17]=1>>[CH2:21]([C:10]1[C:9]([F:11])=[CH:8][CH:7]=[C:6]([F:12])[C:5]=1[OH:4])[CH:16]=[CH2:17]

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 949N,N-DimethylanilineHCID 107496562,5-Difluorophenol allyl ether

生成物 1

HCID 108448632-Allyl-3,6-difluorophenol

反応条件

温度
170 °C

実験手順

The 2,5-difluorophenol allyl ether (13 g) was dissolved in N,N-dimethylaniline (90 ml) and the resulting solution was stirred under a nitrogen gas stream at 170° C. for 5 hr. Then the liquid reaction mixture was poured into a 10% aqueous solution of hydrogen chloride and extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (developing solvent: 7% ethyl acetate/n-hexane) to give 2-allyl-3,6-difluorophenol (7.8 g) as a colorless oil.

後処理

  1. customThen the liquid reaction mixture
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe resulting residue was purified by silica gel column chromatography (developing solvent: 7% ethyl acetate/n-hexane)

出典と根拠

ORDレコード
ord-32e18329d084413c8c3d50c9c45f4cd1
出典データセット
uspto-grants-2001_07
特許番号
US06258811B1

反応ノート

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