HRID128163

反应详情

EQUATION

反应方程式

HRID 128163 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionis added 1.4 g
  2. customevaporated in vacuo to an oil
  3. dissolutionThis oil is dissolved in 150 ml
  4. filtrationof benzene and filtered through Magnesol®
  5. customThe filtrate is evaporated to 50 ml
  6. additionand petroleum ether is added to effect crystallization
  7. filtrationThe product is collected by filtration
  8. customrecrystallized from benzene-petroleum ether with charcoal treatment