Реакция #80687

ord-eb7d6f215aae481d8c9b19d52895372b

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураwhile maintaining the reaction mixture temperature below 10° C
  2. 2
    workup.ADDITIONAfter the addition
  3. 3
    Температураcooled to 10° C.
  4. 4
    ФильтрацияThe resultant aqueous mixture is filtered
  5. 5
    Другоеto obtain a solid which
  6. 6
    Промывкаis washed with water
  7. 7
    Другоеair-dried

Методика

Nitric acid (70% real, 8.3 mL, 0.131 mol) is added to a solution of 1-(2-chloro-4-fluorophenyl)-3-methyl-s-triazine-2,4,6(1H,3H,5H)-trione (32.4 g, 0.119 mol) in concentrated sulfuric acid while maintaining the reaction mixture temperature below 10° C. After the addition is complete, the reaction mixture is stirred at room temperature for 30 minutes, cooled to 10° C. and diluted with ice-water. The resultant aqueous mixture is filtered to obtain a solid which is washed with water and air-dried to give the title product as a white solid (28.5 g, mp 135°-139° C.).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05616706uspto-grants-1997_04