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

HRID 1384071노트

반응식

HRID 1384071 반응식
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]

참가 물질

4

반응물 3

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

생성물 1

HCID 108448632-Allyl-3,6-difluorophenol

반응 조건

온도
170 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-32e18329d084413c8c3d50c9c45f4cd1
출처 데이터셋
uspto-grants-2001_07
특허 번호
US06258811B1

반응 노트

불러오는 중…