4-Nitrophenol → 1-(2-Bromo-1,1,2-trifluoroethoxy)-4-nitrobenzene

HRID 1583282

反応式

HRID 1583282 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[CH:6][CH:5]=1)([O-:3])=[O:2].[OH-].[K+].[Br:13][C:14]([F:18])=[C:15]([F:17])[F:16]>CN(C)C=O>[Br:13][CH:14]([F:18])[C:15]([F:17])([F:16])[O:10][C:7]1[CH:8]=[CH:9][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][CH:6]=1

参加物

5

反応物 3

HCID 9804-NitrophenolHCID 117301-Bromo-1,2,2-trifluoroetheneHCID 14797Potassium Hydroxide

生成物 1

HCID 132284951-(2-Bromo-1,1,2-trifluoroethoxy)-4-nitrobenzene

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
40 °C

実験手順

278 g of 4-nitrophenol and 56 g of potassium hydroxide were dissolved in 800 ml of dimethylformamide, 179 g of bromotrifluoroethylene were fed in, a little at a time, at 40° C., and stirring was then continued for 2 hours at 60° C. The solvent was removed under reduced pressure in a rotary evaporator, the residue was poured into ice-water and extracted with 3×500 ml of methylene chloride, the extract was washed with dilute sodium hydroxide solution and water and dried over Na2SO4, and the solvent was removed. When the residue was distilled, 279.5 g of pure product passed over at 114° C./1.3 mbar.

後処理

  1. customThe solvent was removed under reduced pressure in a rotary evaporator
  2. additionthe residue was poured into ice-water
  3. extractionextracted with 3×500 ml of methylene chloride
  4. washthe extract was washed with dilute sodium hydroxide solution and water
  5. dry with materialdried over Na2SO4
  6. customthe solvent was removed
  7. distillationWhen the residue was distilled
  8. custompassed over at 114° C./1.3 mbar

出典と根拠

ORDレコード
ord-9743f657a1bb436fa06a197d84f451d0
出典データセット
uspto-grants-1985_11
特許番号
US04551448

関連ノート

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