Reacción #3806

ord-633d84603ffe4743a9aba35936f4eeaa

Condiciones de reacción

Temperatura
23°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    ConcentraciónThe mixture was concentrated
  2. 2
    Otrothe residue triturated with 5% aqueous HCl
  3. 3
    Filtraciónthe resulting solid was collected by filtration
  4. 4
    Lavadowashed with water
  5. 5
    Otroto yield the crude product
  6. 6
    OtroThe crude material was recrystallized from ethyl ether-ethanol

Procedimiento

A solution of 2,2'-dithiobisbenzoyl chloride (1.20 g, 3.50 mmol) in 25 mL of dichloromethane was added to a solution of 4-tert-butylaniline (1.04 g, 6.99 mmol) in 8 mL of pyridine at 23° C. The reaction mixture was stirred for 18 hours at 23° C. under nitrogen atmosphere. The mixture was concentrated, the residue triturated with 5% aqueous HCl, and the resulting solid was collected by filtration and washed with water to yield the crude product. The crude material was recrystallized from ethyl ether-ethanol to yield 0.24 g of the title compound, mp 135°-138° C.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05734081uspto-grants-1998_03