تفاعل #74618

ord-257ca3bd31f446f79a741ae7a987f53f

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08541588B2uspto-grants-2013_09