反应详情

12.44 g of 5,6,7,8-tetrahydro-8-oxo-2,4-diphenyl-1-benzopyryliumtetrafluoroborate (32 mmol) is suspended in 80 ml of distilled water and a solution of 25 g of ammonium carbaminate (320 mmol) in 200 ml of distilled water is added with stirring. After stirring at room temperature for 24 h, the solution is extracted by suction via a nutsche, washed with distilled water and dried by suction. The cream-coloured powder is washed in portions with diethyl ether and dried at 50° C. in a vacuum drying cabinet to constant weight: 8.39 g of ivory-coloured product (87.5%) with a melting point of 177-178° C. (decomposition). IR (ATR): The CO valence vibration band can be seen at 1700 cm−1. 1H-NMR (500 MHz, CDCl3): δ=8.09 (d, 2H, o-H of 2-phenyl), 7.79 (s, 1H, H3), 7.56-733 (m, 8H, arom. H), 2.92 (t, 2H, J=5.75 Hz), 2.83 (t, 2H, J=6.56 Hz), 2.10 (p, 2H, J=5.75 Hz, J=6.56 Hz).

1. stirringAfter stirring at room temperature for 24 h
2. extractionthe solution is extracted by suction via a nutsche
3. washwashed with distilled water
4. customdried by suction
5. washThe cream-coloured powder is washed in portions with diethyl ether
6. customdried at 50° C. in a vacuum
7. customdrying cabinet to constant weight