Реакция #63140

ord-f56531faf056450bba8134dfded76144

Уравнение реакции

COc1cc(C)nc(N)n1
2-amino-4-methoxy-6-methylpyrimidine
Sc1ccc(Cl)cc1
4-chlorothiophenol
C=O
formaldehyde
CC(=O)O
acetic acid
COc1cc(C)nc(NCSc2ccc(Cl)cc2)n1
2-[(4-chlorophenylthio)methylamino]-4-methoxy-6-methylpyrimidine

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураare heated
  2. 2
    ФильтрацияThe resultant solution is clarified by filtration
  3. 3
    workup.ADDITIONdiluted with 150 ml of toluene
  4. 4
    Другоеthe solvent is removed in a rotary evaporator
  5. 5
    ДругоеThe residue crystallises
  6. 6
    ДругоеThe melting point is 78°-82° after recrystallisation from hexane

Методика

A mixture of 13.99 g of 2-amino-4-methoxy-6-methylpyrimidine (0.1 mole), 14.8 g of 4-chlorothiophenol (0.1 mole), 9.4 g of aqueous 35% formaldehyde (0.11 mole) and 1 g of acetic acid are heated under reflux for 1 hour in 100 ml of methanol. The resultant solution is clarified by filtration, diluted with 150 ml of toluene and then the solvent is removed in a rotary evaporator. The residue crystallises after standing for some time. The melting point is 78°-82° after recrystallisation from hexane. The yield is 24 g (81% of theory).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04764203uspto-grants-1988_08