تفاعل #162630

ord-1bce316c12b245bfb48278a76c850844

المذيبات

ظروف التفاعل

درجة الحرارة
140°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىto give a yellow suspension
  2. 2
    تركيزThe mixture was concentrated
  3. 3
    workup.DISSOLUTIONThe residue was dissolved in dichloromethane
  4. 4
    غسيلwashed
  5. 5
    تجفيفThe organic phase was dried over MgSO4
  6. 6
    ترشيحfiltered
  7. 7
    تركيزconcentrated

الإجراء التجريبي

In a 2-5 mL microwave vial was placed 8-(6-chloro-2-(4-nitrophenyl)pyrimidin-4-yl)-3-oxa-8-azabicyclo[3.2.1]octane (36, 200 mg, 0.577 mmol) in iPrNH2 (5 mL) to give a yellow suspension. The reaction was heated under microwave irradiation at 140° C. for 3×45 min. The mixture was concentrated. The residue was dissolved in dichloromethane and washed with sat NaHCO3. The organic phase was dried over MgSO4, filtered and concentrated to give the title compound (208 mg, 98%) as a yellow foam. HRMS: For [M+H]+ mass error=0.1 mDa or 0.23 ppm.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08835429B2uspto-grants-2014_09