With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.696-07-1, name is 5-Iodouracil, molecular formula is C4H3IN2O2, molecular weight is 237.9833, as common compound, the synthetic route is as follows.Safety of 5-Iodouracil
To a dry DMF (50 mL) solution of 5-iodouracil 23 (5.00 g, 21 mmol), tetrakis (triphenylphosphine) palladium (0) (1.00 g, 0.87 mmol, 0.04 equiv. ) and copper iodide (0.80 g, 4.2 mmol, 0.2 equiv. ) under a nitrogen atmosphere was added dry DIPEA (7.3 mL, 5.42 g, 42 mmol, 2 equiv. ) and 1-DODECYNE 24 (13.5 ML, 10.48 g, 63 mmol, 3 equiv. ) via syringe with stirring. The initially opaque yellow solution proceeded to change colour on stirring at room temperature to a clear dark yellow solution, and eventually an opaque dark green suspension formed after a couple of hours. The suspension was allowed to react at RT with stirring for 18 h. TLC analysis of the resulting mixture indicated that most of the starting material had reacted, and the presence of a blue fluorescent spot was clearly observed. Dry triethylamine (25 mL) and a further addition of copper iodide (0.80 g) was then made to the suspension, and the resultant reaction mixture heated to 80 C for 6 h with stirring under N2. The suspension was allowed to cool to RT overnight with stirring. The resultant precipitate was collected by suction filtration, and washed consecutively with methanol and DCM. The collected solid was triturated in hot methanol to yield the title COMPOUND 26 as a white insoluble solid of weight 3.79 g (65 % from 23).
At the same time, in my other blogs, there are other synthetic methods of this type of compound,696-07-1, 5-Iodouracil, and friends who are interested can also refer to it.
Reference:
Patent; UNIVERSITY COLLEGE CARDIFF CONSULTANTS LIMITED; REGA FOUNDATION; WO2004/96813; (2004); A1;,
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