[foxthreefour]

I’ve failed to clean up my reaction and as a result I think I have a large amount of hydroxide sludge, maybe a transition metal. What’s worse I’ve used DCM as the extraction solvent and the sludge is effectively being pulled to the bottom very slowly with the DCM as it sinks. It’s like an emusion and is proving insanely hard to separate so I’ve added some toluene to hopefully mix with the DCM and bring it to the surface, leaving the sludge to sink.

I considered acidifying the solution, and with it turning my compound into a salt, removing the organic layers, basifying with NaCO then extracting the oil compound with a new solvent but was worried this may compound the problem and add to the sludge.

Any ideas?

[wildfyr]

Add a bunch of brine and chloroform. Both help reduce emulsions, chlorofmr due it it's worse ability to form micellew, and brine for its better separation properties from organics.

The sludge will hopefully go to the water layer. I hope the toluene doesn't interfere.

[rolnor]

Filter the mixture through Celite, this will remove the sludge.