2-Nitrophenol → 1-(Benzhydryloxy)-2-nitrobenzene

HRID 132589

반응식

HRID 132589 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[OH:10])([O-:3])=[O:2].Br[CH:12]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.[K].C([O-])([O-])=O.[K+].[K+]>CC(C)=O>[CH:12]([O:10][C:5]1[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=1[N+:1]([O-:3])=[O:2])([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1

참가 물질

6

반응물 4

HCID 69472-NitrophenolHCID 11430Potassium CarbonateHCID 236603BromodiphenylmethaneHCID 5462222Potassium

생성물 1

HCID 74341221-(Benzhydryloxy)-2-nitrobenzene수율 39.5%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of o-nitrophenol (2.08 g, 15.0 mmol), 1-[bromo(phenyl)methyl]benzene (3.70 g, 15.0 mmol) and potassium carbonated (K2CO3) (4.14 g, 30.0 mmol) in acetone (60 mL) was kept at reflux temperature for 5 h. The reaction mixture was cooled to room temperature, concentrated in vacuo. The residue was partitioned between dichloromethane (CH2Cl2) and water (H2O), organic layer dried over sodium sulphate (Na2SO4), filtered, concentrated. The residue was purified by silica gel flash chromatography to give subtitled compound (1.81 g).

후처리

  1. temperatureat reflux temperature for 5 h
  2. concentrationconcentrated in vacuo
  3. customThe residue was partitioned between dichloromethane (CH2Cl2) and water (H2O), organic layer
  4. dry with materialdried over sodium sulphate (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe residue was purified by silica gel flash chromatography

출처 및 근거

ORD 기록
ord-079031298525448db5b6e52e03b4a7e2
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07388020B2

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