HRID2220215
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
- 75 °C
PROCEDURE
实验过程
A 15 mL three necked oven dried round bottom flask was cooled under argon and charged with Example 21A (50 mg, 0.12 mmol), Example 236A (47 mg, 0.15 mmol) and toluene (2 mL)/EtOH (1 mL). The mixture was purged with argon for 30 minutes. Pd(PPh3)4 (14 mg, 0.012 mmol) and 2 M Na2CO3 (187 μl, 0.36 mmol were added and the reaction was heated at 75° C. for 2 hours. The resulting mixture was poured into water (10 mL) and extracted with EtOAc (3×10 mL). The combined extracts were dried over Na2SO4, filtered and concentrated. The residue was purified by radial chromatography (2 mm plate, 30% to 50% EtOAc/Hexanes) to give the desired product Example 236B (29 mg, 55%).
WORKUP
后处理
- dry with materialA 15 mL three necked oven dried round bottom flask
- temperaturewas cooled under argon
- customThe mixture was purged with argon for 30 minutes
- extractionextracted with EtOAc (3×10 mL)
- dry with materialThe combined extracts were dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- customThe residue was purified by radial chromatography (2 mm plate, 30% to 50% EtOAc/Hexanes)