HRID238645
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
- 100 °C
PROCEDURE
实验过程
A mixture of (6-fluoro-4-hydroxy-3-vinyl-naphthalen-2-yl)-acetic acid methyl ester (22 mg, 0.084 mmol), 2,5-bis-ethanesulfonyl-pyridine (33 mg, 0.126 mmol), potassium iodide (5 mg), and cesium carbonate (68 mg, 0.21 mmol), N,N-dimethylformamide (0.5 mL) and acetone (1.5 mL) was heated at 100° C. for 30 minutes with microwave irradiation. The mixture was then concentrated in vacuo. The residue was purified by flash column (gradient elution with 0-50% ethyl acetate in petroleum ether) to afford [4-(5-ethanesulfonyl-pyridin-2-yloxy)-6-fluoro-3-vinyl-naphthalen-2-yl]-acetic acid methyl ester (13 mg, 36.1%) as a yellow solid.
WORKUP
后处理
- concentrationThe mixture was then concentrated in vacuo
- customThe residue was purified by flash column (gradient elution with 0-50% ethyl acetate in petroleum ether)