反应详情

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%).

1. additionadded dropwise
2. stirringThe mixture was stirred for 35 minutes
3. customAfter the ice bath was removed
4. stirringthe mixture was further stirred for 2 hours
5. additionAfter the reaction mixture was poured into 100 ml of water, extraction with chloroform
6. washwashing with a saturated saline solution
7. dry with materialdrying over anhydrous sodium sulfate, and concentration
8. customThe residue was purified by silica gel column chromatography
9. washwashed with hexane