HRID418673
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
- 170 °C
PROCEDURE
实验过程
A mixture of 7-chloro-N′,N′-dimethylthieno[3,2-b]pyridine-2-carbohydrazide (237) (798 mg, 3.13 mmol), 2-fluoro-4-nitrophenol (740 mg, 4.70 mmol), K2CO3 (830 mg, 6.26 mmol) and Ph2O (4.2 mL) was stirred in a sealed tube for 12 h at 170° C. The mixture was diluted with DCM, extracted with water, the organic phase dried with anhydrous Na2SO4 and concentrated. The residue was purified by flash chromatography (EtOAc/hexanes 1:1) giving 238 (772.5 mg, 2.05 mmol, 66% yield) as a brown foam. MS (m/z): (M+1) 377.0 (100%).
WORKUP
后处理
- extractionextracted with water
- dry with materialthe organic phase dried with anhydrous Na2SO4
- concentrationconcentrated
- customThe residue was purified by flash chromatography (EtOAc/hexanes 1:1)