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Nitric Acid → HCID 57713304, 화합물

HRID 1983862
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HRID 1983862 반응식
[F:1][C:2]1[CH:3]=[C:4]([C:9]([F:12])([F:11])[F:10])[CH:5]=[C:6]([OH:8])[CH:7]=1.[N+:13]([O-])([OH:15])=[O:14]>C(O)(=O)C.O>[F:1][C:2]1[CH:3]=[C:4]([C:9]([F:10])([F:11])[F:12])[C:5]([N+:13]([O-:15])=[O:14])=[C:6]([OH:8])[CH:7]=1
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참가 물질

5

반응물 2

HCID 944Nitric AcidHCID 27375873-Fluoro-5-(trifluoromethyl)phenol

생성물 1

HCID 57713304HCID 57713304, 화합물수율 21%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매2회

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온도
50 °C

실험 절차

5-Fluoro-3-(trifluoromethyl)phenol (1.27 g) was dissolved in acetic acid (3 ml) and water (1.5 ml), and nitric acid (3.0 ml) was added thereto. The reaction mixture was stirred at 50° C. for 30 minutes. After cooling, water was added to the reaction mixture, and the mixture was extracted with ether. The extract was washed with an aqueous saturated sodium bicarbonate solution and water, dried over magnesium sulfate, and concentrated. The residue was purified by column chromatography (developing solution:ethyl acetate-hexane=1:3) to obtain the title compound as oil (0.33 g, 21%).

후처리

  1. temperatureAfter cooling
  2. extractionthe mixture was extracted with ether
  3. washThe extract was washed with an aqueous saturated sodium bicarbonate solution and water
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated
  6. customThe residue was purified by column chromatography (developing solution:ethyl acetate-hexane=1:3)

출처 및 근거

ORD 기록
ord-2e44993a4b5e42c7a7c5390c7f359712
출처 데이터셋
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07541478B2

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