Question Help with this NaBH4 synthesis please.
- Thread starter Doubleboil
- Start date
Seems you should have went to pH 6. Seems this is a sensitive reaction
??? https://erowid.org/archive/rhodium/chemistry/meth-nabh4.html
??? https://erowid.org/archive/rhodium/chemistry/meth-nabh4.html
@UWe9o12jkied91d Sorry I wasn’t more detailed. Yes I did base the methylamine hcl with NaOH and into methanol. Assuming the steps prior were all correct…. I’m now stuck with the free base oil which I’m hesitant to gas with hcl….
Why? You could perform solvent extraction, add aq. HCl like 20%, optionally add a bit more water, extract the organic phase well, separate it off, heat the water to evaporate gently, once you have about as much water as HCl salt left pour ipa about as much or more than the water and set to crystalize undisturbed, if nothing is showing up evaporate more
- By Doubleboil
After I add the hcl 20%, it will seperate into layers? Taking the organic layer on top and heating it slowly. At what point should I see precipitate? Or it stays an oil and won’t see anything until it begins to crystallise? Because from what I understand, if I was to use hcl gas into it, it should start turning hard?
yes, since rest is water it will separate.You add HCl, add some water, separate solvent mechanically, evaporate some water, crystalize.Your hcl salt will be in the water, dissolved, you will see solids after evaporating most of the water and adding ipOH after a day or
A layer separated out from what? What were you trying to salt in that there's a layer?
- By Doubleboil
When adjusting ph of dcm/oil, as the PH dropped, a new layer formed on top. I know is not the dilute hcl cause the volume is much greater then that.
- By Doubleboil
Yes. The dcm is regent grade. But if this carbon tetrachloride on top, then the organic oil is still in the dcm?