تفاعل #60910

ord-1c0feb97983e42f0819bc2d7cfbe1541

ظروف التفاعل

درجة الحرارة
80°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىdegassed
  2. 2
    أخرىThe solvent was evaporated
  3. 3
    أخرىthe residue was purified by flash chromatography on silica using 0-100% EtOAc in DCM
  4. 4
    أخرىFurther purification by preparative RPBPLC

الإجراء التجريبي

6-[4-(3-Bromophenyl)-1-methyl-1H-imidazol-5-yl]thieno[2,3-d]pyrimidin-4-amine (Example 50) (192 mg) was stirred with zinc cyanide (118 mg) and tetrakis(triphenylphosphine)palladium (116 mg) in DMF (7 mL), degassed, then heated under an inert atmosphere at 80° C. for 20 hours. The solvent was evaporated and the residue was purified by flash chromatography on silica using 0-100% EtOAc in DCM then 0-20% MeOH in DCM as eluent. Further purification by preparative RPBPLC using an MeCN/water/formic acid gradient gave the title compound as a solid (28 mg, 16%);

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07427616B2uspto-grants-2008_09