HRID63625
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
- 150 °C
PROCEDURE
实验过程
A suspension of 6-hydroxy-1-tetralone (3.0 g, 18 mmol), 2-fluoro-6-methylpyridine (2.06 g, 18.5 mmol) and Cs2CO3 (12.1 g, 37.0 mmol) in DMF (150 mL) was stirred at 150° C. in a sealed vessel overnight under N2. The reaction was poured into water (300 mL) and extracted with EtOAc (3×50 mL). Organics were dried (Na2SO4) and concentrated. Purification by silica gel chromatography (PE:EA=5:1) gave 1.2 g (26%) of the title compound as a red oil. [M+H] calc'd for C16H15NO2, 254. found 254.
WORKUP
后处理
- extractionextracted with EtOAc (3×50 mL)
- dry with materialOrganics were dried (Na2SO4)
- concentrationconcentrated
- customPurification by silica gel chromatography (PE:EA=5:1)