반응 #215345

반응 방정식

p-fluorobenzoylacetonitrile

N,N-dimethylacetamide dimethylacetal

→

desired product

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

용매

chloroform

반응 조건

후처리

1. 1
   workup.ADDITIONis added 1.4 g
2. 2
   기타evaporated in vacuo to an oil
3. 3
   workup.DISSOLUTIONThis oil is dissolved in 150 ml
4. 4
   여과of benzene and filtered through Magnesol®
5. 5
   기타The filtrate is evaporated to 50 ml
6. 6
   workup.ADDITIONand petroleum ether is added to effect crystallization
7. 7
   여과The product is collected by filtration
8. 8
   기타recrystallized from benzene-petroleum ether with charcoal treatment

실험 절차

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.

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