I am working with platinum(IV) prodrugs. Most of the synthetic procedures states that after most of DMSO is removed the residue should be treated with methanol and ether, giving the desired compound.
However, in my cases, after precipitating platinum complex with methanol and ether, the residue turns from what seems like a solid into the viscous oil. Thus, I want to know can there be more efficient method to isolate platinum(IV) complexes from the DMSO?
Dear Daniil Spektor did you follow a literature procedure to make your platinum(IV) prodrugs? If yes, what did the authors say about purification of the compounds? Generally simple precipitation does not immediately a very pure compound. You could e.g. repeat the precipitation (redissolve in DMSO and precipitate with diethyl ether again). When you get an oil again, you can try to triturate it with diethyl ether while stirring with a glass rod to convert it into a powder. You can of course also try to recrystallize the crude product e.g. from hot ethanol or acetonitrile.
If you are making a known compound, please follow the procedure systematically. When you prepare a chemical compound most of the time you may not be able to isolate analytically pure product, for which you have to use one of the methods for purification. For solids, best procedure is crystallization or sublimation if the compound is stable. If more than one product is expected use fractional crystallization method. If it is liquid, distilling under vacuo. If you get oil, you may have to wash it several times with solvents such as diethyl ether or pentane (in which your product should not be soluble) to get solid residue. Once you get a solid residue, you should use an appropriate combination of solvents for Re-crystallization. Before that you have to check for its solubility in various solvents. Read more literature to know what best you can do, so that you will not depend on others. This is an opportunity to learn the art of synthesis.
Mr. D. Spektor,
If your compound really carries platinum, it should be solid rather to liquid. Hope you did not filter the precipitate. However, from yours point of conversion of solid to liquid upon addition of methanol and ether, it is to think. One suggestion is - wash the precipitate or obtained viscous liquid with ether under negative temperature condition twice to thrice and you may get the solid (provided if the compound contains desired product).
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