Water → 1H-Inden-1-one, 4-bromo-2,3-dihydro-5-(trifluoromethyl)-

HRID 2406509노트

반응식

HRID 2406509 반응식
[Br:1][C:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:12][CH2:13][C:14]([OH:16])=O.O>FC(F)(F)S(O)(=O)=O>[Br:1][C:2]1[C:7]([C:8]([F:9])([F:10])[F:11])=[CH:6][CH:5]=[C:4]2[C:3]=1[CH2:12][CH2:13][C:14]2=[O:16]

참가 물질

4

반응물 2

HCID 962WaterHCID 53808869Benzenepropanoic acid, 2-bromo-3-(trifluoromethyl)-

생성물 1

HCID 867007731H-Inden-1-one, 4-bromo-2,3-dihydro-5-(trifluoromethyl)-

시약·촉매·용매 1

HCID 62406Trifluoromethanesulfonic acid용매

실험 절차

3-(2-Bromo-3-trifluoromethyl-phenyl)-propionic acid (3.25 g) in trifluoromethane-sulfonic acid (30 ml) is stirred at 75° C. for 2.5 h. After cooling to room temperature, the mixture is poured into water and the resulting mixture is extracted with ethyl acetate. The combined organic extract is washed with aqueous NaHCO3 solution, dried (Na2SO4), and concentrated. The residue is chromatographed on silica gel (cyclohexane/ethyl acetate 90:10→80:20) to afford the title compound. LC (method 5): tR=0.90 min.

후처리

  1. extractionthe resulting mixture is extracted with ethyl acetate
  2. extractionThe combined organic extract
  3. washis washed with aqueous NaHCO3 solution
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated
  6. customThe residue is chromatographed on silica gel (cyclohexane/ethyl acetate 90:10→80:20)

출처 및 근거

ORD 기록
ord-03cd12b569d944b895e291befb69779e
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08809376B2

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