반응 #74618

ord-257ca3bd31f446f79a741ae7a987f53f

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08541588B2uspto-grants-2013_09