Nitric Acid → HCID 14473250、化合物

HRID 238949ノート

反応式

HRID 238949 の反応式
[N+:1]([O-:4])(O)=[O:2].[F:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([O:12][C:13]([F:16])([F:15])[F:14])[CH:7]=1>S(=O)(=O)(O)O>[F:5][C:6]1[CH:11]=[CH:10][C:9]([N+:1]([O-:4])=[O:2])=[C:8]([O:12][C:13]([F:14])([F:15])[F:16])[CH:7]=1

参加物

4

反応物 2

HCID 944Nitric AcidHCID 27772861-Fluoro-3-(trifluoromethoxy)benzene

生成物 1

HCID 14473250HCID 14473250、化合物収率 16%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

反応条件

温度
-10 °C

実験手順

Fuming nitric acid (20 mL) was added dropwise to concentrated sulfuric acid (40 ml) under cooling (−10° C.), and subsequently, 1-fluoro-3-(trifluoromethoxy)benzene (15 g, 83 mmol) was added to the mixture at −10° C., and the mixture was stirred for 0.5 hours. After the mixture was added into ice-water to stop the reaction, it was extracted with dichloromethane. After the obtained organic layer was washed with a 1N aqueous sodium hydroxide solution and water, it was dried with anhydrous sodium sulfate. After filtration, the solution was concentrated and the residue was purified by silica gel column chromatography (100:0-97:3, hexane:ethyl acetate) to give the title compound (3.1 g, 16%) as an oil.

後処理

  1. customthe reaction, it
  2. extractionwas extracted with dichloromethane
  3. washAfter the obtained organic layer was washed with a 1N aqueous sodium hydroxide solution and water, it
  4. dry with materialwas dried with anhydrous sodium sulfate
  5. filtrationAfter filtration
  6. concentrationthe solution was concentrated
  7. customthe residue was purified by silica gel column chromatography (100:0-97:3, hexane:ethyl acetate)

出典と根拠

ORDレコード
ord-9055eb9eb43e47cf84ffecaf8ed26270
出典データセット
uspto-grants-2014_02
特許番号
US08642640B2

反応ノート

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