تفاعل #69551

ord-191f418fb6ab49d39998070494b19864

المذيبات

ظروف التفاعل

درجة الحرارة
60°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.DISTILLATIONthe solvent was directly distilled off under reduced pressure
  2. 2
    أخرىThe residue was purified by silica gel column chromatography (a mixed solvent of n-heptane and ethyl acetate

الإجراء التجريبي

To a dioxane (15 mL) solution of tert-butyl{2-bromo-3-[2,6-dimethoxy-4-(methoxymethyl)phenyl]-6-methoxypyrazolo[5,1-b][1,3]thiazol-7-yl}carbamate (323 mg, 0.612 mmol) were added 2M dimethyl zinc (0.612 mL, 1.22 mmol) and bis(tri-tert-butylphosphine)palladium(0) (15.6 mg, 0.031 mmol), and the mixture was heated at 60° C. for one hour. After the reaction was completed, the solvent was directly distilled off under reduced pressure. The residue was purified by silica gel column chromatography (a mixed solvent of n-heptane and ethyl acetate: n-heptane/ethyl acetate=1/1) to obtain the title compound (205 mg, 0.442 mmol).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08530504B2uspto-grants-2013_09