HRID1970280

反应详情

EQUATION

反应方程式

HRID 1970280 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

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

  1. additionwere added
  2. filtrationfiltered
  3. customorganic layer was separated
  4. concentrationconcentrated
  5. customThe crude material was purified by flash chromatography on 40 g RediSep column