تفاعل #167912

ord-2a30010c88fe4cd29478672b484c4d43

المذيبات

ظروف التفاعل

درجة الحرارة
135°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe solvent is then evaporated off under reduced pressure
  2. 2
    أخرىthe oily residue is chromatographed on a column of silica gel
  3. 3
    غسيلeluting with a stepwise gradient of methanol and aqueous ammonia in dichloromethane (0:0:100 to 2:1:98)

الإجراء التجريبي

A mixture of 0.15 g (0.42 mmol) of 4-[6-chloro-2-(4-chlorophenyl)imidazo[1,2-b]pyridazin-3-yl]pyrid-2-ylamine and 0.36 g (1.7 mmol) of tert-butyl hexahydropyrrolo[3,4-c]pyrrole-2-carboxylate in 7 mL of pentanol is stirred at 135° C. for 20 hours. The solvent is then evaporated off under reduced pressure and the oily residue is chromatographed on a column of silica gel, eluting with a stepwise gradient of methanol and aqueous ammonia in dichloromethane (0:0:100 to 2:1:98). 0.16 g of product is isolated after trituration in diisopropyl ether, filtering off and drying under reduced pressure.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08846676B2uspto-grants-2014_09