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
A mixture of 4-(7-bromo-3,4-dihydroisoquinolin-2(1H)-yl)-6-(4-methylpiperazin-1-yl)pyrimidin-2-amine (22.4 mg, 0.0556 mmol), (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (12.9 mg, 0.0222 mmol, Aldrich, Cat. No. 526460), palladium acetate (2.50 mg, 0.0111 mmol, Aldrich, Cat. No. 379875), cesium carbonate (36.2 mg, 0.111 mmol) and urethane (7.43 mg, 0.0834 mmol, Aldrich, Cat. No. 418331) in 1,4-dioxane (1 mL) was degassed with nitrogen and then heated at 120° C. for 20 h. The reaction mixture was cooled to r.t. and concentrated under reduced pressure. The residue was dissolved in MeOH and purified by RP-HPLC (pH=10) to afford the desired compound. LCMS (M+H)+: m/z=412.2.
WORKUP
后处理
- custom418331) in 1,4-dioxane (1 mL) was degassed with nitrogen
- temperatureThe reaction mixture was cooled to r.t.
- concentrationconcentrated under reduced pressure
- dissolutionThe residue was dissolved in MeOH
- custompurified by RP-HPLC (pH=10)