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Nitric Acid → N-[2-Nitro-4-[1-(trifluoroacetyl)-2-pyrrolidinyl]-5-fluorophenyl]trifluoroacetamide

HRID 13399
ノート
印刷プレビュー

反応式

HRID 13399 の反応式
[N+:1]([O-:4])(O)=[O:2].[F:5][C:6]([F:29])([F:28])[C:7]([NH:9][C:10]1[CH:15]=[CH:14][C:13]([CH:16]2[CH2:20][CH2:19][CH2:18][N:17]2[C:21](=[O:26])[C:22]([F:25])([F:24])[F:23])=[C:12]([F:27])[CH:11]=1)=[O:8]>O>[F:29][C:6]([F:5])([F:28])[C:7]([NH:9][C:10]1[CH:11]=[C:12]([F:27])[C:13]([CH:16]2[CH2:20][CH2:19][CH2:18][N:17]2[C:21](=[O:26])[C:22]([F:23])([F:24])[F:25])=[CH:14][C:15]=1[N+:1]([O-:4])=[O:2])=[O:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 944Nitric AcidHCID 23145429HCID 23145429、化合物

生成物 1

HCID 23145265N-[2-Nitro-4-[1-(trifluoroacetyl)-2-pyrrolidinyl]-5-fluorophenyl]trifluoroacetamide

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

100 ml of fuming nitric acid was added to 28 g of 2,2,2-trifluoro-N-(3-fluoro-4-(1-(trifluoroacetyl)pyrrolidin-2-yl)phenyl)acetamide with cooling with ice, and the reaction liquid was stirred at room temperature for 1 hour. Water with ice was added to the reaction liquid to dilute it, then extracted with ethyl acetate, washed with saturated saline, and dried with anhydrous magnesium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=10/1) to obtain the entitled compound as a yellow oily substance.

後処理

  1. temperaturewith cooling with ice
  2. customthe reaction liquid
  3. additionto dilute it
  4. extractionextracted with ethyl acetate
  5. washwashed with saturated saline
  6. dry with materialdried with anhydrous magnesium sulfate
  7. customThe solvent was evaporated away under reduced pressure
  8. customthe resulting residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=10/1)
  9. customto obtain the entitled compound as a yellow oily substance

出典と根拠

ORDレコード
ord-30ca783781e344fda6f5bdc143843efa
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07728025B2

反応ノート

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