反応 #653655

ord-8c9ce8dc6e014aa1a6fe3202a06a5152

溶媒

反応条件

温度
4°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.STIRRINGThe reaction mixture was stirred at 23° C. for 15 hours
  2. 2
    その他precipitates
  3. 3
    その他formed
  4. 4
    その他The precipitates (triethylamine.HBr)
  5. 5
    ろ過were filtered out
  6. 6
    濃縮the filtrate was concentrated to dryness
  7. 7
    その他Then the crude reaction mixture
  8. 8
    その他was purified by column chromatography (SiO2, hexane/CH2Cl2=5/1)

実験手順

A mixture of 5-acenaphthylamine (1.0 g, 6 mmol) and triethylamine (0.76 g, 7.5 mmol) in toluene (50 mL) was stirred at 4° C., and 4-tert-butylbenzyl-bromide (1.36 g, 6 mmol) was added in slowly. The reaction mixture was stirred at 23° C. for 15 hours and precipitates formed. The precipitates (triethylamine.HBr) were filtered out; the filtrate was concentrated to dryness. Then the crude reaction mixture was purified by column chromatography (SiO2, hexane/CH2Cl2=5/1). N-(5-acenaphthyl)-4-tert-butylbenzylamine (1.67 g, an oil) was obtained.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06174924B1uspto-grants-2001_01