HRID2379697
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
- 0 °C
PROCEDURE
实验过程
144.3 g (0.6 mol) of 2-chloro-3,4-dimethyl-5-pivaloylaminopyridine are dissolved in 2.9 1 of abs. THF and the solution is treated under argon at -78° C. with 127 ml of a 10.4N solution of n-BuLl in n-hexane (1.32 mmol). The mixture is stirred at 0° C. for 3 h, 129.8 ml (0.6 mol) of 2,2-diethoxyacetophenone are slowly added at -78° C. and the mixture is stirred at room temperature overnight. It is then added to water and extracted 3 times with ethyl acetate, dried and concentrated on a rotary evaporator. The purity is sufficient for further reaction. After chromatography, 180.5 g (67%) of the title compound are obtained. M.p.: 133° C.
WORKUP
后处理
- stirringthe mixture is stirred at room temperature overnight
- extractionextracted 3 times with ethyl acetate
- customdried
- concentrationconcentrated on a rotary evaporator
- customThe purity is sufficient for further reaction