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

HRID 2381159ノート

反応式

HRID 2381159 の反応式
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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-760b9606c1cc434d9867470cb9e9bc16
出典データセット
uspto-grants-2012_09
特許番号
US08258158B2

反応ノート

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