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
- 150 °C
PROCEDURE
实验过程
A microwave tube is charged with [4-(6-bromobenzo[b]thiophen-2-yl)-pyrimidin-2-yl]-[3-(4-methylpiperazin-1-yl)-propyl]-amine (0.070 g, 0.16 mmol), 1.5 equivalent of 2-(1H-indol-3-yl)acetamide (0.041 g, 0.24 mmol), 4 mol % of tris(dibenzylideneacetone)dipalladium(0) (5.8 mg, 0.0063 mmol), 8 mol % of Xantphos (7.3 mg, 0.013 mmol), 1.5 equivalent of cesium carbonate (77 mg, 0.24 mmol) and acetonitrile (2 mL). The reaction is sealed and heated under microwave condition at 150° C. for 5 minutes, cooled down, filtered and then evaporated to furnish a red oil. This material is subjected to reverse phase purification, eluting with 20-95% CH3CN/0.01 M NH4HCO3 in water using a C18 Xterra column, to provide the title compound as a pale yellow solid (23 mg, 26% yield). ES+(m/z) 540 [M+H].
WORKUP
后处理
- customThe reaction is sealed
- temperaturecooled down
- filtrationfiltered
- customevaporated
- customto furnish a red oil
- customphase purification
- washeluting with 20-95% CH3CN/0.01 M NH4HCO3 in water using a C18 Xterra column