반응 #354683

ord-f466e7f3e608468bbec349a29fcb6b95

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONA mixture of 36.8 g
  2. 2
    workup.DISTILLATIONsteam distilled
  3. 3
    기타to remove the excess o-xylene
  4. 4
    기타The water was decanted from the pot residue
  5. 5
    여과the remaining solid filtered
  6. 6
    세척washed with acetone
  7. 7
    기타dried
  8. 8
    기타to yield 58.1 g
  9. 9
    기타Recrystallization from benzene
  10. 10
    기타gave an analytically pure sample, m.p. 235°-236°

실험 절차

A mixture of 36.8 g. (0.20 mole) of cyanuric chloride, 88.0 g. (0.66 mole) of anhydrous aluminum chloride and 250 ml. of o-xylene was heated at 45°C for 1.5 hours. After cooling to room temperature, the mixture was poured into ice water, and then steam distilled to remove the excess o-xylene. The water was decanted from the pot residue and the remaining solid filtered, washed with acetone and dried to yield 58.1 g. of product, m.p. 220°-230°. Recrystallization from benzene gave an analytically pure sample, m.p. 235°-236°.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US03943133uspto-grants-1976_03