反应详情

Dissolve 120 mg 1-[1-(3,3-dimethyl-2-oxobutyl)-6-methoxy-1H-indazol-3-yl]-2-methylprop-1-en-1-yl dimethyl phosphate from Example 1 in 0.75 mL anhydrous DCM. Cool the solution in an ice bath under nitrogen. Add 108 mg trimethylsilyl bromide and let the reaction mixture sit at room temperature for 2.5 hours. Remove solvent under reduced pressure. The residue was dissolved in a mixture of MeCN and water and purified by RP-HPLC using 10-100% MeCN gradient with about 0.05% TFA to give the title compound as a colorless solid after lyophilization. This reaction can also be carried out in MeCN. The title compound can also be purified by recrystallization in anhydrous MeCN.

1. temperatureCool the solution in an ice bath under nitrogen
2. custompurified by RP-HPLC