反应详情

温度

90 °C

Under N2 atmosphere, 0.18 parts of 5-(7-dibutylamino-9H-fluoren-2-yl)-thiophene-2-carbaldehyde (12a), 0.05 parts of cyanoacetic acid, and 0.017 parts of piperidine were added into acetonitrile, followed by stirring and mixing. Then, the reaction mixture was heated to 90° C. and reacted for 6 hours. After the reaction mixture was cooled to room temperature, the reaction mixture was filtrated to obtain a solid. Then, the solid was washed with water, ether, and acetonitrile sequentially to obtain a dark red solid. Finally, this crude was purified with column chromatography method by using dichloromethane/methanol co-solvent as an eluent, to obtain a compound (13a) of the present example. This compound was in a form of a dark red solid, and the yield of this compound was 73%.

1. additionmixing
2. customreacted for 6 hours
3. temperatureAfter the reaction mixture was cooled to room temperature
4. filtrationthe reaction mixture was filtrated
5. customto obtain a solid
6. washThen, the solid was washed with water, ether, and acetonitrile sequentially
7. customto obtain a dark red solid
8. customFinally, this crude was purified with column chromatography method