HRID411228
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
A mixture of 2,6-dimethyl-3-aminopyridine (0.85 g) and diethyl ethoxymethylenemalonate (1.53 g) is heated at 135° C. in xylene (30 mL) for 2 h allowing for removal of ethanol. After the solvent is removed, the mixture is suspended in diphenyl ether (15 mL). The mixture is then heated to reflux with removal of ethanol for 30 min. The reaction mixture is cooled to room temperature and hexanes (20 mL) is added. The resulting precipitate is filtered, washed with diethyl ether (2×10 mL) and dried to give 0.5 g (30%) of the title compound as a brown solid. Physical chracteristics: MS (ESI+) m/z 247 (M+H)+; 1H NMR (DMSO) δ 8.67, 7.97,4.38, 2.85,2.67, 1.40.
WORKUP
后处理
- customallowing for removal of ethanol
- customAfter the solvent is removed
- temperatureThe mixture is then heated
- temperatureto reflux with removal of ethanol for 30 min
- additionhexanes (20 mL) is added
- filtrationThe resulting precipitate is filtered
- washwashed with diethyl ether (2×10 mL)
- customdried