반응 #483914

ord-89f6527309c7417da998df8ccd1ab7c7

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the mixture is heated
  2. 2
    온도to reflux temperature
  3. 3
    온도After a reaction time of 5 hours the clear, brownish solution is cooled
  4. 4
    여과clarified by filtration through 100 g of silica gel
  5. 5
    기타The yellow solution is evaporated
  6. 6
    기타the residue is recrystallized from hexane/toluene

실험 절차

23.8 g (0.06 mol) of 2-(2,4-dihydroxyphenyl)-4,6-bis-(2,4-dimethylphenyl)-1,3,5-triazine (prepared as described in U.S. Pat. No. 3,244,708 Example 16) are suspended in 300 ml of xylene. 12.1 g (0.09 mol) of 97% butyl glycidyl ether and 0.75 g (0.006 mol) of dimethylbenzylamine are added to this suspension, and the mixture is heated to reflux temperature. After a reaction time of 5 hours the clear, brownish solution is cooled and clarified by filtration through 100 g of silica gel. The yellow solution is evaporated and the residue is recrystallized from hexane/toluene. This gives 27.3 g of pale yellow crystals of 2-[2-hydroxy-4(3-butoxy-2-hydroxypropyloxy)-phenyl]-4,6-bis(2,4-dimethylphenyl)-1,3,5-triazin (=86% yield). Melting point: 80-83° C. (Compound 1).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06608122B1uspto-grants-2003_08