反应详情

温度

40 °C

In 3 ml of N,N-dimethylformamide, 0.13 g (1.01 mmol) of tetracyanoethylene was dissolved. With stirring under ice cooling, 0.4 g (0.95 mmol) of [3-benzyloxy-4-[2-(thiophene-2-yl)vinyl]phenyl]dibutyl amine was dissolved in 1 ml of N,N-dimethylformamide and added dropwise. The mixture was stirred for 40 minutes and further stirred with heating at 40° C. overnight. 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 ethanol to give 157 mg of a black crystal having a mp of 125-130° C. (yield: 31.7%).

1. additionadded dropwise
2. stirringThe mixture was stirred for 40 minutes
3. stirringfurther stirred
4. washwashing with a saturated saline solution
5. dry with materialdrying over anhydrous sodium sulfate, and concentration
6. customThe residue was purified by silica gel column chromatography
7. washwashed with ethanol