Reacción #74618

ord-257ca3bd31f446f79a741ae7a987f53f

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroThe reaction mixture immediately turned yellow and a precipitate was formed
  2. 2
    Concentraciónthe mixture was concentrated in vacuo
  3. 3
    workup.STIRRINGwater (75 mL) and stirred for 15 minutes
  4. 4
    FiltraciónThe resulting solid was filtered
  5. 5
    Otrodried in vacuo

Procedimiento

4-Aminopyrimidine (1.0 g, 10.5 mmol) and DABCO™ (1.18 g, 10.5 mmol) were added concurrently to a solution of 3-chloro-4-fluorobenzenesulfonyl chloride (1.25 mL, 10.0 mmol) in anhydrous acetonitrile (49 mL). The reaction mixture immediately turned yellow and a precipitate was formed. After stirring for 16 hours, the mixture was concentrated in vacuo. The crude material was suspended in ethyl acetate (75 mL) and water (75 mL) and stirred for 15 minutes. The resulting solid was filtered and dried in vacuo to afford the title compound, 0.83 g, 27% yield.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08541588B2uspto-grants-2013_09