反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
To a solution of (S)-ethyl 2-tert-butoxy-2-(7-(4-chlorophenyl)-2-(2-chloropyridin-4-yl)-5-methylbenzo[d]thiazol-6-yl)acetate (35.0 mg, 0.066 mmol) and 1-methyl-3-(trimethylstannyl)-1H-indazole (24.0 mg, 0.079 mmol) in dioxane (0.9 mL) was added Pd(PPh3)4 (4.0 mg, 3.03×10−3 mmol) and CuI (4.0 mg, 0.018 mmol). The reaction was degassed for 5 minutes with N2 and then heated at 100° C. overnight. After cooling, the reaction mixture was diluted with EtOAc, extracted with H2O, brine, dried over Na2SO4, filtered and concentrated and purified by flash column chromatography (silica gel, 0 to 70% ethyl acetate/hexanes) to give the desired product. LCMS-ESI+ (m/z): [M+H]+ calcd for C35H34ClN4O3S: 625.2; found: 625.3.
WORKUP
后处理
- customThe reaction was degassed for 5 minutes with N2
- temperatureAfter cooling
- additionthe reaction mixture was diluted with EtOAc
- extractionextracted with H2O, brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- custompurified by flash column chromatography (silica gel, 0 to 70% ethyl acetate/hexanes)