反応 #1048

ord-bf89635c7d584db89b9fd587daa3d2c0

反応条件

温度
100°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度gradually raised in temperature to 200° C.
  2. 2
    workup.STIRRINGfurther stirred for 2 hours
  3. 3
    温度This was then cooled to room temperature
  4. 4
    その他the product was purified by silica gel column chromatography (chloroform:methanol:water (2% acetic acid)=65:35:5)

実験手順

A mixture of 500 mg of 4-(4-fluorophenyl) methylaniline and 445 mg of bis(2-chloroethyl)amine hydrochloride was stirred at 100° C. for 2 hours, then gradually raised in temperature to 200° C. and then further stirred for 2 hours. This was then cooled to room temperature, then the product was purified by silica gel column chromatography (chloroform:methanol:water (2% acetic acid)=65:35:5) to obtain the above-referenced compound (5) in an amount of 503 mg (yield of 75%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05723475uspto-grants-1998_03