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
PROCEDURE
实验过程
To a solution of 4-((4-chloro-5-iodopyrimidin-2-yl)amino)benzonitrile (J12, 100 mg) and tert-butyl(4-pentynyl)carbamate (77 mg) in N,N-dimethylformamide (3 mL), bis(triphenylphosphine)palladium(II) dichloride (20 mg), triethylamine (195 μL) and copper(I) iodide (11 mg) were added at room temperature, and the mixture was stirred at the same temperature for 1 hour. To the reaction mixture, saturated aqueous ammonium chloride and ethyl acetate were added. The organic layer was separated, washed with saturated aqueous sodium chloride, and then dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The obtained solid matter was washed with a mixture of hexane and ethyl acetate (5:1), and then air-dried to obtain tert-butyl (5-(4-chloro-2-((4-cyanophenyl)amino)pyrimidin-5-yl)-4-pentyn-1-yl)carbamate (T5, 73 mg) as pale yellow solid.
WORKUP
后处理
- customThe organic layer was separated
- washwashed with saturated aqueous sodium chloride
- dry with materialdried over anhydrous sodium sulfate
- customthe solvent was evaporated under reduced pressure
- washThe obtained solid matter was washed with a mixture of hexane and ethyl acetate (5:1)
- customair-dried