反応 #1596980

ord-7175792667384f51a8a90f4e13afcaee

反応方程式

O
water
NCCc1ccccc1
2-phenylethylamine
O=[N+]([O-])c1ccccc1F
2-fluoronitrobenzene
O=C([O-])[O-].[K+].[K+]
potassium carbonate
O=[N+]([O-])c1ccccc1NCCc1ccccc1
orange crystals
収率 98.0%
O=[N+]([O-])c1ccccc1NCCc1ccccc1
N-Phenylethyl-2-nitroaniline
収率 98.0%

溶媒

反応条件

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

後処理

  1. 1
    温度The mixture was then cooled to ambient temperature
  2. 2
    その他resulted in the precipitation of a light orange compound
  3. 3
    ろ過The solid was recovered by filtration
  4. 4
    その他dried

実験手順

A mass of 4.8 g (0.04 mol) of 2-phenylethylamine was added dropwise, at ambient temperature, to a mixture of 5.6 g (0.04 mol) of 2-fluoronitrobenzene and 11.06 g (0.08 mol) of anhydrous potassium carbonate in 30 ml of DMSO. The mixture was heated at 100° C. for 3 hours. The mixture was then cooled to ambient temperature and was added to 100 ml of water, which resulted in the precipitation of a light orange compound. The solid was recovered by filtration and dried using a desiccator at reduced pressure. A mass of 9.4 g of orange crystals was obtained with a yield of 98%. The melting point found was coherent with the theoretical value, i.e. 64-66° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08211662B2uspto-grants-2012_07