HRID1970280
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
- 65 °C
PROCEDURE
实验过程
100 ml RBF was charged with (R)-2′-bromo-7′-iodo-5H-spiro[oxazole-4,9′-xanthen]-2-amine (1.5 g, 3.28 mmol), pyrimidin-5-ylboronic acid (0.488 g, 3.94 mmol), tetrakis(triphenylphosphine)palladium(0) (0.284 g, 0.246 mmol). DME (23.44 mL) followed by sodium carbonate (4.92 mL, 9.85 mmol) (2M solution) were added and the mixture was heated at 65° C. for 24 h. The mixture was diluted with water and EtOAc, filtered and organic layer was separated and concentrated. The crude material was purified by flash chromatography on 40 g RediSep column using 5-70% gradient of DCM/MeOH/NH4OH in DCM to give (S)-2′-bromo-7′-(pyrimidin-5-yl)-5H-spiro[oxazole-4,9′-xanthen]-2-amine.
WORKUP
后处理
- additionwere added
- filtrationfiltered
- customorganic layer was separated
- concentrationconcentrated
- customThe crude material was purified by flash chromatography on 40 g RediSep column