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Nitronium tetrafluoroborate → HCID 21084116、化合物

HRID 347839
ノート
印刷プレビュー

反応式

HRID 347839 の反応式
[CH3:1][O:2][CH2:3][C:4]1[CH:13]=[C:7]2[CH:8]=[CH:9][CH:10]=[C:11]([Br:12])[N:6]2[N:5]=1.F[B-](F)(F)F.[O:19]=[N+:20]=[O:21]>C(#N)C>[CH3:1][O:2][CH2:3][C:4]1[C:13]([N+:20]([O-:21])=[O:19])=[C:7]2[CH:8]=[CH:9][CH:10]=[C:11]([Br:12])[N:6]2[N:5]=1
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 11073463Nitronium tetrafluoroborateHCID 21084117HCID 21084117、化合物

生成物 1

HCID 21084116HCID 21084116、化合物収率 46%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a solution of (7-bromopyrazolo[1,5-a]pyridin-2-yl)methyl methyl ether (1.0 g) dissolved in acetonitrile (20 mL) was added nitronium tetrafluoroborate (606 mg) while stirring on ice. The obtained reaction mixture was added to ice water, extracted with ethyl acetate and then washed with water and brine. The obtained organic extract was dried over anhydrous magnesium sulfate and filtered, the solvent was evaporated under reduced pressure, the residue was purified by silica gel column chromatography and the title compound (546 mg) was obtained as light yellow crystals from the n-hexane:ethyl acetate (5:1) fraction.

後処理

  1. customThe obtained reaction mixture
  2. extractionextracted with ethyl acetate
  3. washwashed with water and brine
  4. extractionThe obtained organic extract
  5. dry with materialwas dried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. customthe solvent was evaporated under reduced pressure
  8. customthe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-1467342e5c1e4742a8df54eaba2e2583
出典データセット
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07176216B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート