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Boron trifluoride etherate → 1-Azido-1-methylcyclopentane

HRID 246582
ノート
印刷プレビュー

反応式

HRID 246582 の反応式
B(F)(F)F.CCOCC.[CH3:10][C:11]1(O)[CH2:15][CH2:14][CH2:13][CH2:12]1.C[Si]([N:21]=[N+:22]=[N-:23])(C)C>C1(C)C=CC=CC=1>[N:21]([C:11]1([CH3:10])[CH2:15][CH2:14][CH2:13][CH2:12]1)=[N+:22]=[N-:23]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8000Boron trifluoride etherateHCID 738301-MethylcyclopentanolHCID 78378Azidotrimethylsilane

生成物 1

HCID 866779941-Azido-1-methylcyclopentane収率 110.8%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

BF3.Et2O (934 mg, 6.23 mmol) was added drop-wise at 20° C. to a stirred solution of 1-methylcyclopentanol (520 mg, 5.19 mmol) and trimethylsilyl azide (716 mg, 6.23 mmol) in 6 mL of toluene. Then the solution was stirred at room temperature for 16 hours. The organic phase was washed with a 10% solution of NaHCO3 (10 mL), water (5 mL) and brine (5 mL), and dried over anhydrous sodium sulfate. The drying agent was removed by filtration and the solvent was evaporated at 35° C. under reduced pressure to give 1-azido-1-methylcyclopentane (720 mg) as a crude product. It was used directly in the next step without further purification.

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

後処理

  1. washThe organic phase was washed with a 10% solution of NaHCO3 (10 mL), water (5 mL) and brine (5 mL)
  2. dry with materialdried over anhydrous sodium sulfate
  3. customThe drying agent was removed by filtration
  4. customthe solvent was evaporated at 35° C. under reduced pressure

出典と根拠

ORDレコード
ord-a713a77f9ac642e1885baae772931151
出典データセット
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08658646B2

反応ノート

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