تفاعل #560841

ord-c3626ddc923647bab10de00cd13c2f77

المذيبات

ظروف التفاعل

درجة الحرارة
105°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىbefore evacuating
  2. 2
    workup.ADDITIONwas added
  3. 3
    أخرىconsumption of the starting material
  4. 4
    درجة الحرارةthe reaction mixture was cooled to room temperature
  5. 5
    أخرىthe volatiles were removed under reduced pressure

الإجراء التجريبي

To a 25 mL microwave vial was added Bis(tri-tert-butylphosphine) palladium (0) (101 mg, 0.198 mmol) and N-(4-(3-bromopyridin-2-yloxy)phenyl)pyridin-2-amine hydrochloride (750 mg, 1.981 mmol) before evacuating and backfilling with nitrogen (2×). After addition of Dioxane (5.659 ml), N-cyclohexyl-N-methylcyclohexanamine (0.840 ml, 3.96 mmol), and 3,4-dihydro-2H-pyran (666 mg, 7.92 mmol) was added and the mixture was heated to 105° C. Following complete consumption of the starting material, the reaction mixture was cooled to room temperature and the volatiles were removed under reduced pressure. Following silica gel chromatography, the title compound was obtained as a racemic mixture. MS (ESI, pos. ion) m/z: 346.0. IC50 (uM) 0.064.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08637500B2uspto-grants-2014_01