HRID128163
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
- -10 °C
PROCEDURE
实验过程
To a solution of 1.6 g. of p-fluorobenzoylacetonitrile [Pihl et al., Reakts. Sposobnost Org. Soedin. Tartu. Gos. Univ., 5 (1), 27, (1968)] in 30 ml. of chloroform, cooled to -10° C., is added 1.4 g. of N,N-dimethylacetamide dimethylacetal. The reaction mixture is stirred at -10° C. for 2 hours and then evaporated in vacuo to an oil. This oil is dissolved in 150 ml. of benzene and filtered through Magnesol®. The filtrate is evaporated to 50 ml. and petroleum ether is added to effect crystallization. The product is collected by filtration and then recrystallized from benzene-petroleum ether with charcoal treatment giving the desired product.
WORKUP
后处理
- additionis added 1.4 g
- customevaporated in vacuo to an oil
- dissolutionThis oil is dissolved in 150 ml
- filtrationof benzene and filtered through Magnesol®
- customThe filtrate is evaporated to 50 ml
- additionand petroleum ether is added to effect crystallization
- filtrationThe product is collected by filtration
- customrecrystallized from benzene-petroleum ether with charcoal treatment