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Azidotrimethylsilane → 1-(2-Azido-2-methylpropyl)-4-(trifluoromethyl)benzene

HRID 244953
ノート
印刷プレビュー

反応式

HRID 244953 の反応式
[CH3:1][C:2](O)([CH3:14])[CH2:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]([F:13])([F:12])[F:11])=[CH:6][CH:5]=1.C[Si]([N:20]=[N+:21]=[N-:22])(C)C>C(Cl)Cl>[N:20]([C:2]([CH3:14])([CH3:1])[CH2:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]([F:13])([F:12])[F:11])=[CH:6][CH:5]=1)=[N+:21]=[N-:22]
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 78378AzidotrimethylsilaneHCID 651450142-Methyl-1-(4-(trifluoromethyl)phenyl)propan-2-ol

生成物 1

HCID 866974731-(2-Azido-2-methylpropyl)-4-(trifluoromethyl)benzene収率 86.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

26.3 g of 2-methyl-1-(4-(trifluoromethyl)phenyl)propan-2-ol was dissolved in 400 mL of methylene chloride, and 25 mL (0.19 mol) of trimethylsilyl azide and 24 mL (0.19 mol) of boron trifluoride diethyl ether complex were added dropwise under cooling with ice. The reaction mixture was stirred at room temperature for 20 hours. After completion of the reaction, the reaction mixture was washed with saturated aqueous sodium hydrogen carbonate and with saturated aqueous sodium chloride successively, dried over anhydrous sodium sulfate and filtered, and the filtrate was concentrated under reduced pressure to give 25.4 g of the desired product.

後処理

  1. temperatureunder cooling with ice
  2. customAfter completion of the reaction
  3. washthe reaction mixture was washed with saturated aqueous sodium hydrogen carbonate and with saturated aqueous sodium chloride successively
  4. dry with materialdried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-7c0bfcfffe2043caa376f8bc7bfa3f62
出典データセット
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08658686B2

反応ノート

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