反応 #74832

反応方程式

p-fluorobenzoylacetonitrile

N,N-dimethylacetamide dimethylacetal

→

desired product

3-Dimethylamino-2-(p-fluorobenzoyl)crotononitrile

溶媒

chloroform

反応条件

後処理

1. 1
   workup.ADDITIONis added 1.4 g
2. 2
   その他the evaporated in vacuo to an oil
3. 3
   workup.DISSOLUTIONThis oil is dissolved in 150 ml
4. 4
   ろ過of benzene and filtered through magnesol
5. 5
   その他The filtrate is evaporated to 50 ml
6. 6
   workup.ADDITIONand petroleum ether is added to effect crystallization
7. 7
   ろ過The product is collected by filtration
8. 8
   その他recrystallized from benzene-petroleum ether with charcoal treatment

実験手順

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 the 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.

出典