反应详情

温度

50 °C

In 7 ml of N,N-dimethylformamide, 235 mg (1.83 mmol) of tetracyanoethylene was dissolved. With stirring under ice cooling, 600 mg (1.75 mmol) of dibutyl[3-methoxy-4-[2-(thiophene-2-yl)vinyl]phenyl]amine was dissolved in 2 ml of N,N-dimethylformamide and added dropwise. The mixture was stirred for 1.5 hours. After the ice bath was removed, the mixture was stirred at room temperature for 1 hour and further stirred with heating at 50° C. overnight. After the reaction mixture was poured into 80 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 methanol to give 324 mg of a dark reddish crystal having a mp of 189-192° C. (yield: 41.8%).

1. additionadded dropwise
2. stirringThe mixture was stirred for 1.5 hours
3. customAfter the ice bath was removed
4. stirringthe mixture was stirred at room temperature for 1 hour
5. stirringfurther stirred
6. additionAfter the reaction mixture was poured into 80 ml of water, extraction with chloroform
7. washwashing with a saturated saline solution
8. dry with materialdrying over anhydrous sodium sulfate, and concentration
9. customThe residue was purified by silica gel column chromatography
10. washwashed with methanol
11. customto give 324 mg of a dark reddish crystal