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
PROCEDURE
实验过程
N NaOH (81 μL) was added to a solution containing methyl 5-fluoromethoxypyridine-2-carboxylate (50 mg) in THF/water (2 mL, 3/1), and the mixture was stirred at RT for 10 min. Water (1 mL) was added to the reaction solution, followed by further stirring for 20 min. The reaction solution was made acidic with 5 N hydrochloric acid. EtOAc and a saturated NaCl solution were added to the reaction solution, and the organic layer was separated. The organic layer was dried over anhydrous MgSO4, and the insoluble matter was separated by filtration. The filtrate was concentrated to obtain the title compound (22.6 mg). 1H-NMR (CDCl3) δ (ppm): 5.81 (d, J=53.2 Hz, 2H), 7.61 (ddd, J=0.8, 2.8, 8.8 Hz, 1H), 8.25 (d, J=0.8, 8.8 Hz, 1H), 8.42 (d, J=2.4 Hz, 1H).
WORKUP
后处理
- stirringby further stirring for 20 min
- customthe organic layer was separated
- dry with materialThe organic layer was dried over anhydrous MgSO4
- customthe insoluble matter was separated by filtration
- concentrationThe filtrate was concentrated