p-Fluoronitrobenzene → Nitro-4-(2,2,2-trifluoro-1-methyl-ethoxy)-benzene

HRID 2381159

반응식

HRID 2381159 반응식
F[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][CH:3]=1.[F:11][C:12]([F:17])([F:16])[CH:13]([OH:15])[CH3:14].C([O-])([O-])=O.[Cs+].[Cs+]>C(#N)C>[N+:8]([C:5]1[CH:6]=[CH:7][C:2]([O:15][CH:13]([CH3:14])[C:12]([F:17])([F:16])[F:11])=[CH:3][CH:4]=1)([O-:10])=[O:9]

참가 물질

5

반응물 3

HCID 9590p-FluoronitrobenzeneHCID 97741,1,1-Trifluoro-2-propanolHCID 10796Cesium carbonate

생성물 1

HCID 66577895Nitro-4-(2,2,2-trifluoro-1-methyl-ethoxy)-benzene수율 95.4%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a solution of 1-fluoro-4-nitro-benzene (4.24 g) and (rac)-1,1,1-trifluoro-propan-2-ol (4.563 g) in acetonitile (50 ml) under an argon atmosphere was added at RT Cs2CO3 (13.04 g) and the mixture was refluxed for 10 h. It was then acidified with diluted aqueous HCL and partitioned between ethyl acetate and water. The layers were separated, dried over Na2SO4 and the solvent was then evaporated off to give (rac)-1-nitro-4-(2,2,2-trifluoro-1-methyl-ethoxy)-benzene as brown oil (6.74 g) that was used without further purification.

후처리

  1. temperaturethe mixture was refluxed for 10 h
  2. custompartitioned between ethyl acetate and water
  3. customThe layers were separated
  4. dry with materialdried over Na2SO4
  5. customthe solvent was then evaporated off

출처 및 근거

ORD 기록
ord-760b9606c1cc434d9867470cb9e9bc16
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08258158B2

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