反応 #64197

ord-790cc1ed03c34f3892fab8140e2d2c08

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度heated to 25°
  2. 2
    抽出the mixture is extracted twice with ethyl acetate
  3. 3
    洗浄washed neutral with water
  4. 4
    乾燥dried over sodium sulfate
  5. 5
    濃縮concentrated to dryness under vacuum

実験手順

5 g of 4-[1-(1,2,4-triazolyl)methyl]benzonitrile is dissolved in 100 ml of tetrahydrofuran and combined at -50° with 19.8 ml of 1.5-molar solution of lithium diisopropylamide in tetrahydrofuran, stirred for 0.5 hour, further stirred with 4.25 g of adamantanone for 1 hour at -70°, and heated to 25°. Then water is added, the mixture is extracted twice with ethyl acetate, washed neutral with water, dried over sodium sulfate, and concentrated to dryness under vacuum, yielding 9 g of crude 4-(2-hydroxyadamant-2-yl-1(1,2,4-triazolyl)methyl]benzonitrile.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05411982uspto-grants-1995_05