Aney 0 Posted December 13, 2018 how to deal with sticky mass which produced during organic synthesis ? 0 Share this post Link to post Share on other sites
hypervalent_iodine 1233 Posted December 13, 2018 Could you elaborate? Is this the final product following work up? Deal with how? 0 Share this post Link to post Share on other sites
Aney 0 Posted December 13, 2018 it is building block for synthesis of the final products I want to make it as powder to complete my work any idea for helping ??? 0 Share this post Link to post Share on other sites
hypervalent_iodine 1233 Posted December 13, 2018 Is it meant to be a powder? Sometimes you just have to work with what you’ve got. It shouldn’t matter too much that it’s a sticky solid, unless the fact that it’s sticky is because it contains impurities. 1 Share this post Link to post Share on other sites
Sensei 814 Posted December 13, 2018 (edited) 8 hours ago, Aney said: how to deal with sticky mass which produced during organic synthesis ? If you meant "how to separate chemical compounds?", you should start from reading this article and its links: https://en.wikipedia.org/wiki/Separation_process It should give you brief idea which procedures are available. Edited December 13, 2018 by Sensei 1 Share this post Link to post Share on other sites
Aney 0 Posted December 14, 2018 9 hours ago, hypervalent_iodine said: Is it meant to be a powder? Sometimes you just have to work with what you’ve got. It shouldn’t matter too much that it’s a sticky solid, unless the fact that it’s sticky is because it contains impurities. It is recommended to be solid powder, because of my fearing that impurities make it as sticky mass not powder .. 10 hours ago, Sensei said: If you meant "how to separate chemical compounds?", you should start from reading this article and its links: https://en.wikipedia.org/wiki/Separation_process It should give you brief idea which procedures are available. O. K 0 Share this post Link to post Share on other sites
hypervalent_iodine 1233 Posted December 14, 2018 Have you run any NMR or GCMS? 0 Share this post Link to post Share on other sites
Aney 0 Posted December 14, 2018 1 hour ago, hypervalent_iodine said: Have you run any NMR or GCMS? No .. 0 Share this post Link to post Share on other sites
hypervalent_iodine 1233 Posted December 15, 2018 I would suggest you do that so you can figure out what you have first. 1 Share this post Link to post Share on other sites
John Cuthber 3549 Posted December 15, 2018 There are two options. Use the stuff as it is to make your final product (in which case the product will need cleaning up) Clean up this intermediate- which will give you a product that's cleaner- but will still need cleaning up to get a pure material. The second course of action will probably give a better product, but the yield will be lower. It's more or less traditional in chemistry that you have that trade -off. You can have high purity or high yield, but not (usually) both 1 Share this post Link to post Share on other sites
Aney 0 Posted December 16, 2018 On 12/15/2018 at 4:49 AM, John Cuthber said: There are two options. Use the stuff as it is to make your final product (in which case the product will need cleaning up) Clean up this intermediate- which will give you a product that's cleaner- but will still need cleaning up to get a pure material. The second course of action will probably give a better product, but the yield will be lower. It's more or less traditional in chemistry that you have that trade -off. You can have high purity or high yield, but not (usually) both Nice speech .. On 12/14/2018 at 4:40 PM, hypervalent_iodine said: Have you run any NMR or GCMS? No .. 0 Share this post Link to post Share on other sites
hypervalent_iodine 1233 Posted December 16, 2018 Also worth noting that some reactions tolerate impurities better than others, so I would again recommend that you at least figure out what’s in there first. Can I ask what you’re making? 1 Share this post Link to post Share on other sites
Aney 0 Posted December 16, 2018 1 hour ago, hypervalent_iodine said: Also worth noting that some reactions tolerate impurities better than others, so I would again recommend that you at least figure out what’s in there first. Can I ask what you’re making? I will go ahead to the next reaction using the same sticky mass because NMR and MS take long time to be done .. 0 Share this post Link to post Share on other sites
hypervalent_iodine 1233 Posted December 16, 2018 That is not a great attitude. NMR and MS really take very little time, assuming you have access to the facilities. Certainly a lot less compared to how long it may take you to redo your reaction if it doesn’t work out because you didn’t want to invest an hour or two in doing some very standard checks. Where has this sticky mass of yours come from? Did you make it? 0 Share this post Link to post Share on other sites
John Cuthber 3549 Posted December 17, 2018 13 hours ago, hypervalent_iodine said: That is not a great attitude. NMR and MS really take very little time, assuming you have access to the facilities And if that assumption is invalid...? 0 Share this post Link to post Share on other sites
hypervalent_iodine 1233 Posted December 17, 2018 Their previous post indicates that they have access, but I am not sure if it is administered as a walk-up or as a service operated by a technician. The latter would likely have longer wait times for results. Regardless, I think in the long run you end up wasting more time proceeding with a reaction if you don’t actually know for sure what is going into it. Depending on how precious this compound is and how complicated the reaction they’re doing is, you could probably get away with doing a test run on small scale and seeing how the reaction tolerates it. Even then, figuring out if it worked could be made more difficult by the added impurities, if the ‘sticky mass’ is even the compound they want and not just a decomposed mess, or something stemming from a bad synthesis. 0 Share this post Link to post Share on other sites
BabcockHall 43 Posted December 18, 2018 I hesitate to jump in without knowing more. On occasion a sticky mass can be made more tractable through trituration. Perhaps a different purification technique would be more suitable. 0 Share this post Link to post Share on other sites