تفاعل #70545

ord-65c1901d151e45e48f0b1f53084003e2

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تركيزThe mixture was concentrated
  2. 2
    workup.ADDITIONthe residue was mixed with water (60 mL)
  3. 3
    استخلاصextracted with CH2Cl2
  4. 4
    أخرىThe crude product was purified on a silica gel column
  5. 5
    غسيلeluting with 7.5% methanol in CH2Cl2 saturated with NH3

الإجراء التجريبي

A solution of 4-fluoro-2-methoxy-1-nitrobenzene (1.711 g, 10 mmol), N,N-dimethylpiperidin-4-amine (1.410 g, 11.00 mmol) and N-ethyl-N-isopropylpropan-2-amine (3.48 mL, 20.00 mmol) in anhydrous N,N-dimethylformamide (25 mL) was stirred at 70° C. overnight. The mixture was concentrated and the residue was mixed with water (60 mL), adjusted to pH 12, then extracted with CH2Cl2. The crude product was purified on a silica gel column eluting with 7.5% methanol in CH2Cl2 saturated with NH3 to provide the title compound. (ESI+) m/e 280.1 (M+H)+.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08536180B2uspto-grants-2013_09