반응 #172504

반응 방정식

tetracyanoethylene

dibutyl(3-methoxyphenyl)amine

→

black crystal

수율 77.2%

2-cyano-3-(4-dibutylamino-2-methoxyphenyl)-2-butenedinitrile

수율 77.2%

용매

N,N-dimethylformamide

N,N-dimethylformamide

반응 조건

후처리

1. 1
   workup.ADDITIONadded dropwise
2. 2
   workup.STIRRINGThe mixture was stirred for 35 minutes
3. 3
   기타After the ice bath was removed
4. 4
   workup.STIRRINGthe mixture was further stirred for 2 hours
5. 5
   workup.ADDITIONAfter the reaction mixture was poured into 100 ml of water, extraction with chloroform
6. 6
   세척washing with a saturated saline solution
7. 7
   건조drying over anhydrous sodium sulfate, and concentration
8. 8
   기타The residue was purified by silica gel column chromatography
9. 9
   세척washed with hexane

실험 절차

In 8 ml of N,N-dimethylformamide, 0.5 g (3.9 mmol) of tetracyanoethylene was dissolved. With stirring under ice cooling, 0.8 g (3.4 mmol) of dibutyl(3-methoxyphenyl)amine was dissolved in 2 ml of N,N-dimethylformamide and added dropwise. The mixture was stirred for 35 minutes. After the ice bath was removed, the mixture was further stirred for 2 hours. After the reaction mixture was poured into 100 ml of water, extraction with chloroform, washing with a saturated saline solution, drying over anhydrous sodium sulfate, and concentration were performed. The residue was purified by silica gel column chromatography and washed with hexane to give 0.88 g of a black crystal having a mp of 86° C. (yield: 77.2%).

출처