反应详情

温度

120 °C

4-bromo-5-methylthiophene-2-carbaldehyde (11.00 g, 53.6 mmol) was treated with 2,2-dimethoxyethanamine (17.5 ml, 161 mmol) and the mixture stirred at 120° C. for 12 hours. The reaction was poured into water (50 ml) and stirred for 1 hour and extracted with ethyl acetate. The organic layer was washed (2×) with an aqueous saturated solution of sodium bicarbonate, then with water and then brine. The organic layer was then dried with sodium sulfate, concentrated under reduced pressure and placed under a vacuum line to give (E)-N-((4-bromo-5-methylthiophen-2-yl)methylene)-2,2-dimethoxyethanamine.

1. stirringstirred for 1 hour
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed (2×) with an aqueous saturated solution of sodium bicarbonate
4. dry with materialThe organic layer was then dried with sodium sulfate
5. concentrationconcentrated under reduced pressure