Nitric Acid → HCID 14473250, 화합물

HRID 238949노트

반응식

HRID 238949 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 14473250HCID 14473250, 화합물수율 16%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

반응 조건

온도
-10 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-9055eb9eb43e47cf84ffecaf8ed26270
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08642640B2

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