For those who is interested. I've tried this route. Overall I can confirm it works, except reaction conditions. Temperature and timing were not even close as it's stated in video. Though, in the video they use Iodo-ketone. That's a significant difference.
So, the test run I got 50g of bromine substituted 4-MPF. That was dissolved in 250ml of ethylacetate
than 100ml of aq. 38% methylamine was added. and left to stir at room temp:
After about 30min. not much had changed:
At this moment I decided to heat things up . Not higher about 50-55C.
One hour later:
It was showing some movement. And was left for another hour.
Then basically the steps were the same as in video. Ethylacetate layer with freebase was separated, washed with water, HCL added dropwise until slightly acidic pH. Then acetone poured and filtered.
And that gave raw product. Rather nice at first sight, but should be further purified, of course.
So, the test run I got 50g of bromine substituted 4-MPF. That was dissolved in 250ml of ethylacetate
than 100ml of aq. 38% methylamine was added. and left to stir at room temp:
After about 30min. not much had changed:
At this moment I decided to heat things up . Not higher about 50-55C.
One hour later:
It was showing some movement. And was left for another hour.
Then basically the steps were the same as in video. Ethylacetate layer with freebase was separated, washed with water, HCL added dropwise until slightly acidic pH. Then acetone poured and filtered.
And that gave raw product. Rather nice at first sight, but should be further purified, of course.
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