تفاعل #54159

ord-3f5c1017e42d4c01a4553abe59481e5b

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    غسيلAfter rinsing with nitrogen, 150 ml of acetone
  2. 2
    workup.ADDITIONwere added
  3. 3
    درجة الحرارةupon heating the reaction mixture for a longth of time
  4. 4
    درجة الحرارةunder reflux
  5. 5
    أخرىAfter completion of the reaction
  6. 6
    استخلاصThe organic layer was extracted three times with methylene chloride
  7. 7
    غسيلafter which the combined extracts were washed
  8. 8
    أخرىdried
  9. 9
    أخرىAfter concentration of the organic layer by evaporation a product
  10. 10
    أخرىwas obtained which
  11. 11
    أخرىcrystallized out after a length of time (melting point 18°-20° C.)

الإجراء التجريبي

In a 500 ml-three-necked flask 4.8 g (0.01 mole) of the 2-chloro-4,6-dilauroxy-s-triazine prepared above, were mixed with 2.6 g (0.01 mole) of 2,6-diphenyl hydroquinone. After rinsing with nitrogen, 150 ml of acetone were added, followed by adding dropwise, with vigorous stilling, 0.4 g (0.01 mole) of NaOH dissolved in 7 ml of water, at 20° C. The solution then assumed an orange-yellow color, which largely disappeared upon heating the reaction mixture for a longth of time under reflux. After completion of the reaction, the contents of the flask were poured into 100 ml of ice water containing 2 ml of hydrochloric acid. The organic layer was extracted three times with methylene chloride, after which the combined extracts were washed and dried. After concentration of the organic layer by evaporation a product was obtained which crystallized out after a length of time (melting point 18°-20° C.).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04147659uspto-grants-1979_04