How to remove TiCl4 from the organic reaction mixture containing peptide product?

TiCl4 is often used as a Lewis acid catalyst in organic reactions. Removing it from the reaction mixture is important to avoid unwanted side reactions and improve the quality of the final product. Here are a few methods to remove TiCl4 from an organic reaction mixture containing a peptide product:

Extractive workup: TiCl4 is soluble in polar organic solvents such as methanol or ethanol, but insoluble in non-polar solvents like dichloromethane (DCM). You can extract the TiCl4-containing organic layer into a separate container and then add an equal volume of methanol or ethanol. The polar solvent will dissolve the TiCl4, while the peptide will remain in the original organic layer. The two layers can then be separated, and the organic layer containing the peptide can be dried over anhydrous sodium sulfate to remove any residual moisture.

Column chromatography: Another option is to purify the peptide by column chromatography. The reaction mixture can be loaded onto a silica gel column and eluted with a suitable solvent system (e.g., DCM/MeOH or DCM/EtOAc). The peptide should elute as a separate peak from the TiCl4. The final peptide-containing fraction can then be dried over anhydrous sodium sulfate.

Basic workup: If the reaction mixture is acidic, you can neutralize it with a strong base (e.g., sodium hydroxide or sodium carbonate) to convert the TiCl4 into the insoluble Ti(OH)4. The mixture can then be filtered to remove the solid, and the filtrate can be dried over anhydrous sodium sulfate to remove any residual moisture.

It's important to keep in mind that the specific method you choose may depend on the solubility and reactivity of the peptide, as well as the conditions of the reaction mixture. In general, it's a good idea to consult the literature or consult with an expert to determine the best method for your specific situation.

Ahmad Al Khraisat

To separate the peptide from the organic mixture containing TiCl4 and remove the TiCl4, you can consider the following steps:

Wash the organic mixture with aqueous sodium chloride solution: This step can help to remove residual salts, such as TiCl4, from the organic mixture. The organic layer can be separated from the aqueous layer using a separatory funnel. The organic layer should be washed with a fresh sodium chloride solution and the process should be repeated a few times until the aqueous layer is no longer contaminated with salts.

Remove the organic solvent: You can use a rotary evaporator to remove the organic solvent, such as DCM, from the organic mixture. You should remove the solvent under reduced pressure and at low temperature to prevent degradation of the peptide.

Precipitate the peptide: To remove any residual salts and organic solvents, you can precipitate the peptide by adding an appropriate amount of cold alcohol, such as ethanol or isopropanol, to the solution. The mixture should be cooled overnight in a refrigerator to allow the peptide to precipitate.

Collect the peptide: The peptide can be collected by centrifugation and then washed with cold alcohol several times to remove any residual salts and organic solvents.

Dry the peptide: The peptide can be dried using a speed-vac or other evaporation methods to remove any residual alcohol.

Note that this is a general outline and the specific conditions and methods may vary depending on the nature of your peptide and the conditions of your experiment. It's always advisable to consult the literature and perform a trial run to optimize the conditions for your specific case.

Goran Benedeković

Of all the earlier suggestions, only Geir Bjorklund's proposal (3rd basic workup) is the safest. I do not recommend column purification or evaporation of the reaction solution without first destroying the TiCl4.

https://www.youtube.com/watch?v=bR_LAr_mOCw

Balachandar Sundarrajan

Thank you one and all for your valuable suggestions Geir Bjorklund Ahmad Al Khraisat Goran Benedeković

I may work according to the safest way which is suitable for my reaction condition. I am eExpecting your suggestions throughout all my discussions.

Thanks

Dr. S. Balachandar

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