反应详情

温度

105 °C

Charge a round bottom flask with (1R,2R)-2-methyl-cyclopropanecarboxylic acid (3,4-dibromo-isothiazol-5-yl)-amide (2.55; g, 7.49; mmol), 2-methyl-5-trimethylstannanyl-2H-indazole (2.21; g, 7.49; mmol) and lithium chloride (0.95; g, 22.48; mmol) in 1,4-dioxane (19.2; mL). Purge with nitrogen for 20; min, add tetrakis(triphenylphosphine) palladium (1.31; g, 1.12; mmol) and heat at 105° C. for 48; h. Directly load reaction mixture onto a silica gel column and purify by gradient eluting from 0:100; to 100:0; ethyl acetate:iso-hexane to give the title compound (1.25; g, 43%). MS (m/z): 391, 393; (M+1).

1. customPurge with nitrogen for 20
2. additionmin, add tetrakis(triphenylphosphine) palladium (1.31; g, 1.12; mmol)
3. customDirectly load reaction mixture onto a silica gel column
4. custompurify
5. washby gradient eluting from 0:100