反応 #51634

ord-14089d6065474121a1b9c499e0722165

溶媒

反応条件

温度
0°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度the mixture is heated
  2. 2
    温度under reflux until completion of the reaction (5-12 hours)
  3. 3
    ろ過is filtered off
  4. 4
    洗浄washed with water
  5. 5
    その他The crude material is purified by usual silica gel chromatography

実験手順

A solution of bromo(4-nitrophenyl)acetaldehyde and potassium thiocyanate (1.2 equivalents) in methanol is stirred at room temperature for 1 hour. The cyclohexylamine (1,05 equivalents) is added drop-wise and the mixture is heated under reflux until completion of the reaction (5-12 hours). After cooling to 0° C. the precipitate is filtered off and washed with water. The crude material is purified by usual silica gel chromatography to give the desired compound.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06852720B2uspto-grants-2005_02