反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 120 °C
PROCEDURE
实验过程
3-Fluoro-1-(phenylsulfonyl)-6-(trimethylstannanyl)-1H-indazol-4-amine (660 mg), Pd(PPh3)4 (168 mg) and 4-bromo-2-methyl-1-(phenylsulfonyl)-1H-pyrrolo[2,3-b]pyridine (613 mg) were weighed into a microwave vial and DMF (10 ml) was added. The mixture was heated to 120° C. overnight. The mixture was then cooled to RT and the solvent was removed in vacuo. The crude material was dried in a vacuum oven overnight. The resulting dark brown oil was purified by FlashMaster II. The crude material was dissolved in chloroform and added to the top of 2×100 g silica SPE cartridges that were subsequently eluted with 0-100% ethyl acetate:cyclohexane over 80 min. The product-containing fractions were combined and the solvent removed in vacuo to give the title compound, 357 mg as a cream solid.
WORKUP
后处理
- additionwas added
- temperatureThe mixture was then cooled to RT
- customthe solvent was removed in vacuo
- dry with materialThe crude material was dried in a vacuum oven overnight
- customThe resulting dark brown oil was purified by FlashMaster II
- dissolutionThe crude material was dissolved in chloroform
- additionadded to the top of 2×100 g silica SPE cartridges that
- washwere subsequently eluted with 0-100% ethyl acetate
- customthe solvent removed in vacuo