Reacción #1946560

ord-45bf06e15d644313a0a134eda93238f9

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otrowas prepared, to which
  2. 2
    Temperaturaheated on a steam bath for 23 hrs
  3. 3
    Temperaturacooled
  4. 4
    ExtracciónThe mixture was extracted with methylene chloride
  5. 5
    Lavadothe extracts were washed with water
  6. 6
    Secadodried over magnesium sulfate
  7. 7
    Concentraciónconcentrated
  8. 8
    Otroto crystallize on standing
  9. 9
    Otrowas used without further purification

Procedimiento

A mixture of 114.95 g (356.5 mmol) of N,N-di-n-butyl-N′-(3-methoxybenzoyl)thiourea (compound 1-24), 31.37 g (784.2 mmol) of sodium hydroxide, and 350 ml of water was prepared, to which was added 40.42 g (427.8 mmol) of chloroacetic acid. The mixture was stirred and heated on a steam bath for 23 hrs, then cooled. The mixture was extracted with methylene chloride, and the extracts were washed with water, dried over magnesium sulfate, and concentrated. The oily residue began to crystallize on standing. The yield of thiazole was 100.8 g and was used without further purification.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US06528223B1uspto-grants-2003_03