反応 #74618

ord-257ca3bd31f446f79a741ae7a987f53f

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The reaction mixture immediately turned yellow and a precipitate was formed
  2. 2
    濃縮the mixture was concentrated in vacuo
  3. 3
    workup.STIRRINGwater (75 mL) and stirred for 15 minutes
  4. 4
    ろ過The resulting solid was filtered
  5. 5
    その他dried in vacuo

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08541588B2uspto-grants-2013_09