反应详情

In a stream of argon, in tetrahydrofuran was dissolved 3.0 g (0.97 mmol) of dibutyl[4-[2-(thiophene-2-yl)vinyl]phenyl]amine. To this mixture, 9.0 ml of n-butyllithium (1.6 M solution in hexane) (14.4 mmol) was added dropwise under cooling. After the mixture was stirred for 1 hour, 0.87 g (11.9 mmol) of N,N-dimethylformamide was added dropwise thereto. After 20 minutes, the temperature was allowed to rise and 30 ml of water was added dropwise. Tetrahydrofuran was evaporated off. Extraction with chloroform, drying over anhydrous sodium sulfate, and concentration were performed. The residual liquid was purified by silica gel column chromatography to give 3.12 g of a reddish orange oily matter (yield: 95.5%).

1. temperatureunder cooling
2. waitAfter 20 minutes
3. customTetrahydrofuran was evaporated off
4. extractionExtraction with chloroform
5. dry with materialdrying over anhydrous sodium sulfate, and concentration
6. customThe residual liquid was purified by silica gel column chromatography
7. customto give 3.12 g of a reddish orange oily matter (yield: 95.5%)