Реакция #93043

ord-5226c88d1c5549e8b4879011a276065a

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеThe cooled reaction mixture
  2. 2
    Экстракцияextracted with ether (3×100 ml.)
  3. 3
    ПромывкаThe combined ether fractions were washed with 10% sodium hydroxide solution (2×30 ml.)
  4. 4
    СушкаThe ether solution was dried (Na2SO4)
  5. 5
    Другоеthe solvent evaporated
  6. 6
    Другоеto give a dark oil
  7. 7
    ДругоеTwo crystallizations (petroleum ether)
  8. 8
    Другоеgave 1.91 g

Методика

A stirred solution of methyl 5-chloro-2-nitro-benzoate (17.0 g., 0.079 mole) and the potassium salt of 2,4,6-trichlorophenol (18.6 g., 0.079 mole) in dimethyl sulfoxide (100 ml.) was heated at 90° C. for 17 hours. The cooled reaction mixture was diluted with water (500 ml.) and then extracted with ether (3×100 ml.). The combined ether fractions were washed with 10% sodium hydroxide solution (2×30 ml.) and then with a saturated aqueous chloride solution. The ether solution was dried (Na2SO4) and the solvent evaporated to give a dark oil. Two crystallizations (petroleum ether) gave 1.91 g. of a pale yellow solid, m.p. 101°-103° C.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: USRE032243uspto-grants-1986_09