تفاعل #746282

ord-58e384b3446a4a7aaa4b35a0f80dddbb

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
90°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرى4×2 hours
  2. 2
    أخرىat 130° C.
  3. 3
    أخرىfollowed by 1×8 hours at 130° C
  4. 4
    أخرىThe crude product was partially purified by column chromatography
  5. 5
    غسيلeluting with 10% EtOAc in heptane

الإجراء التجريبي

2-Bromo-6-phenyl-pyridine (13) (100 mg, 0.43 mmol), K2CO3 (117 mg, 0.85 mmol) in acetone (2 mL) was added 3-bromothiophenol and the reaction mixture was heated in a CEM Discover microwave for 1×30 minutes at 90° C., then 4×2 hours at 130° C., followed by 1×8 hours at 130° C. The crude product was partially purified by column chromatography eluting with 10% EtOAc in heptane to give the title compound. Yield: 100 mg, 68%; LC-MS tr 1.97 min; HPLC Purity: 55%; MS (ES+) m/z 342, 344 (M+H)

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08080567B2uspto-grants-2011_12