Reacción #1350589

ord-1457830cd9ea443bbca17272e72d3e21

Condiciones de reacción

Temperatura
0°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    TemperaturaThe reaction mixture was heated at 90° C. for 3 h
  2. 2
    Filtraciónthe precipitate was filtered off with suction
  3. 3
    Lavadowashed with methylene chloride
  4. 4
    workup.DISSOLUTIONThe precipitate was then dissolved in ethyl acetate
  5. 5
    Extracciónextracted with sodium bicarbonate solution
  6. 6
    LavadoAfter washing
  7. 7
    Otrodrying
  8. 8
    Otrothe product was obtained

Procedimiento

56 g of N-(2-methyl-3-methoxycarbonylphenyl)thiourea (0.25 mol) were dissolved in 2 l of chlorobenzene, and the mixture was cooled to 0° C. 40 g of bromine (0.25 mol) in 100 ml of chlorobenzene were then added dropwise. The reaction mixture was heated at 90° C. for 3 h, and the precipitate was filtered off with suction and washed with methylene chloride. The precipitate was then dissolved in ethyl acetate and extracted with sodium bicarbonate solution. After washing and drying, the product was obtained by stripping off the solvent. Yield: 43 g (80%).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US06541423B1uspto-grants-2003_04