반응 #5853

ord-8640071052634bebb681ae075425f7b2

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The thus-formed mixture was then refluxed
  2. 2
    온도under heating for 10 hours
  3. 3
    온도to cool
  4. 4
    기타the insoluble substance was removed by filtration
  5. 5
    세척The thus-obtained filtrate was washed with water
  6. 6
    농축concentrated for the purpose
  7. 7
    기타of recovering the solvent and unreacted raw materials
  8. 8
    기타to obtain a slightly yellow crystal
  9. 9
    기타The crystal was then recrystallized from acetone

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05246810uspto-grants-1993_09