Synthetic Route of 696-07-1, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 696-07-1 as follows.
Step 1 . Preparation of 1 -benzhydryl-5-iodo-pyrimidine-2,4-dione 5-lodouracil (0.10 g, 0.42 mmol) was suspended in dry MeCN (2.1 mL) and Nu, Omicron- bis(trimethylsilyl)acetamide (0.25 mL, 1 .05 mmol) was added under nitrogen atmosphere. When the reaction mixture turned clear, bromodiphenyl methane (0.15 g, 0.63 mmol) and a catalytic amount of l2 were added and the reaction mixture was heated at 84 C for 4 hrs. After cooling to room temperature, the mixture was concentrated under reduced pressure, diluted with EtOAc and washed with water. The aqueous phase was extracted with EtOAc (3 x 15 mL), the combined organic layers were washed with brine, dried over Na2SO4 and the solvent was removed under reduced pressure. The crude was purified by column chromatography using a Teledyne ISCO apparatus (cyclohexane:EtOAc 60:40) to afford the title compound (0.15 g, 87%) as white solid. 1H NMR (400 MHz, CDCI3): delta 7.02 (s, 1 H), 7.14-7.18 (m, 4H), 7.38-7.45 (m, 6H), 7.46 (s, 1 H), 8.58 (s, 1 H). MS (ESI) m/z: 405 [M-H]+.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,696-07-1, its application will become more common.
Reference:
Patent; FONDAZIONE ISTITUTO ITALIANO DI TECNOLOGIA; THE REGENTS OF THE UNIVERSITY OF CALIFORNIA; UNIVERSITA’ DEGLI STUDI DI PARMA; PIOMELLI, Daniele; REALINI, Natalia; MOR, Marco; PAGLIUCA, Chiara; PIZZIRANI, Daniela; SCARPELLI, Rita; BANDIERA, Tiziano; WO2013/178576; (2013); A1;,
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