反応 #5853

ord-8640071052634bebb681ae075425f7b2

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The thus-formed mixture was then refluxed
  2. 2
    温度under heating for 10 hours
  3. 3
    温度to cool
  4. 4
    その他the insoluble substance was removed by filtration
  5. 5
    洗浄The thus-obtained filtrate was washed with water
  6. 6
    濃縮concentrated for the purpose
  7. 7
    その他of recovering the solvent and unreacted raw materials
  8. 8
    その他to obtain a slightly yellow crystal
  9. 9
    その他The crystal was then recrystallized from acetone

実験手順

11.4 g (0.03 mole) of N,N'-bis-(2,6-diisopropylphenyl) guanidine, 5.7 g (0.033 mole) of α,α-dichloro-m-xylene and 2.1 g (0.015 mole) of anhydrous potassium carbonate were added to 50 ml of xylene. The thus-formed mixture was then refluxed under heating for 10 hours. After the mixture had been allowed to cool, the insoluble substance was removed by filtration. The thus-obtained filtrate was washed with water and then concentrated for the purpose of recovering the solvent and unreacted raw materials to obtain a slightly yellow crystal. The crystal was then recrystallized from acetone to obtain 5.1 g of white powder.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05246810uspto-grants-1993_09