反应详情

温度

130 °C

To a solution of crude (S)—N-(1-(3-(4-chloro-1-methyl-3-(methylsulfonamido)-1H-indazol-7-yl)-6-((2-hydroxyethyl)(methyl)amino)pyridin-2-yl)-2-(3,5-difluorophenyl)ethyl)-2,2,2-trifluoroacetamide (57E) in EtOH (1 mL) was added aqueous 2M lithium hydroxide (0.4 mL). The reaction was heated at 130° C. in a microwave reactor for 5 minutes. Upon cooling, aqueous 2N HCl was added until the solution became slightly acidic (pH 4-5). The reaction mixture was then concentrated and taken up in equal volumes of EtOAc and saturated aqueous NaHCO3. The organic layer was collected and the aqueous layer was extracted with a second volume of EtOAc. The combined organic layers were dried over Na2SO4, filtered, concentrated in vacuo, and used without further purification. MS (m/z) 565.09 [M+H]+.

1. temperatureUpon cooling
2. concentrationThe reaction mixture was then concentrated
3. customThe organic layer was collected
4. extractionthe aqueous layer was extracted with a second volume of EtOAc
5. dry with materialThe combined organic layers were dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customused without further purification