Reaktion #69552

Reaktionsgleichung

dioxane

tert-butyl{2-bromo-3-[2,6-dimethoxy-4-(methoxymethyl)phenyl]-6-methoxypyrazolo[5,1-b][1,3]thiazol-7-yl}carbamate

diethyl zinc

→

title compound

tert-Butyl{3-[2,6-dimethoxy-4-(methoxymethyl)phenyl]-2-ethyl-6-methoxymethylpyrazolo[5,1-b][1,3]thiazol-7-yl}carbamate

Lösungsmittel

n-heptane ethyl acetate

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

To a dioxane (5 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 (118 mg, 0.224 mmol), 1M diethyl zinc (0.448 mL, 0.448 mmol) and bis(tri-tert-butylphosphine)palladium(0) (5.70 mg, 0.011 mmol) were added, 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 (84 mg, 0.176 mmol).

Quelle