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Nitric Acid → HCID 57713304、化合物

HRID 1983862
ノート
印刷プレビュー

反応式

HRID 1983862 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

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

生成物 1

HCID 57713304HCID 57713304、化合物収率 21%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒2 回

反応条件

温度
50 °C

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-2e44993a4b5e42c7a7c5390c7f359712
出典データセット
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07541478B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート