تفاعل #52130

ord-baa520823cef4fca827501002f305f40

المذيبات

ظروف التفاعل

درجة الحرارة
70°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe reaction mixture was cooled to room temperature
  2. 2
    أخرىquenched with water
  3. 3
    استخلاصIt was then extracted with methylene chloride
  4. 4
    أخرىthe organic layer separated
  5. 5
    غسيلwashed with water
  6. 6
    أخرىdried
  7. 7
    تركيزconcentrated
  8. 8
    أخرىto give a crude product
  9. 9
    أخرىThe crude product was crystallized from acetone

الإجراء التجريبي

A mixture of 0.9 gm of 2-chloro-4,6-bis(4-phenoxyphenyl)-1,3,5-triazine, 0.24 gm of m-cresol and 0.4 gm AlCl3 in 5 ml chlorobenzene was heated to 70° C. under nitrogen and efficient stirring. After about 4 hr at 70° C., the reaction mixture was analyzed by HPLC, which showed the formation of a new product, and almost disappearance of the starting triazine. The reaction mixture was cooled to room temperature and quenched with water. It was then extracted with methylene chloride, and the organic layer separated, washed with water, dried, and concentrated to give a crude product. The crude product was crystallized from acetone to give pure 2-(2-hydroxy-4-methylphenyl)-4,6-bis(4-phenoxyphenyl)-1,3,5-triazine identified by HPLC, NMR and mass spectroscopy.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06855269B2uspto-grants-2005_02