Ok SWIM attempted the wacker in DMF with no apparent success.
She mixed palladium, benzo, in DMF then dripped in 160g safrole. Then let stir for 7 hours. After was a very dark red substance.
Then was put in freezer because it was 11PM and SWIM had to go to bed.
Next day she pulled it out of the freezer, very thick syrup like substance and the hydroquinone was very visible. Before she did the acid wash she ran it through several coffee filters.
Then it was dumped into a 4L sep funnel along with the 1.5L slightly acidic water. Then it was shaken to mix but the entire sep funnel then turned black from the hydroquinone sticking it the inner surface she presumes. She then shook the sep funnel vigorously and it helped clear it up to determine the layers. Let sit for 20 minutes. She then could see the upper water layer, then also the oraganic lower layer. Lower layer was black, and the top layer a light blood red watery substance. So she assumed to drain off the black layer and leave the upper water layer. When she tried to drain it clogged with the hydroquinone. So she then ran it all through more coffee filters until it was able to drain off. then the upper water layer was washed with first 100ml DCM wash. She could see the oil falling right out of the water into the bottom. it was a light red clear oil. She did this 3 times for a total of 3X100 ml dcm washes. Then all the washes were added together and washed twice with 2X150ml NaOH. That pulled all the remaining hydroquinone out, it was very visible the dark crap went to the top, and the oil fell to the bottom. The upper dark crap layers were tossed.
Then after all that she had almost a full 500ml flask full of this red blood like substance. She set up for vac distillation but the DCM kept jumping to the receiving flask so she distilled off the dcm without vac. all the dcm came over at around 50-60 degrees. There seemed to be about 200-300 ml dcm. Then she turned the vac on. And more substance started coming over at around 100 degrees. Then when it hit 140 degrees she removed the receiving flask and dumped it into a jar. Now this fraction was light red pink. then there was about 30 gram left of this dark dark red with a hint of green substance. Now nothing is distilling anymore and her ghetto hot plate setup is a bitch to regulate (hot plate/stirrer with tin foil tent). the temp now is climbing up and hits 170 degrees and she could see vapors but the temp blasted up to 180 degrees so she pulled it apart and killed the vac worried she would destroy the ketone at that temp. She also noticed a few drops were in the receiving flask and they had a hint of green.
After all this she weighed the distilling flask and realized there was only 30 grams of liquid. That does not correlate with brightstars 100 gram ketone. So she chalked this up to a FAIL.
Now she isnt giving up but needs help. Next step is buying a good heating mantle with good temp control and magnetic stirrer.
Also a note when she distilled the sassy oil, between 100-140 degrees oil was coming over. She is now thinking her safrole isnt pure? Want to test it but hard finding conc. sulfuric acid.
She mixed palladium, benzo, in DMF then dripped in 160g safrole. Then let stir for 7 hours. After was a very dark red substance.
Then was put in freezer because it was 11PM and SWIM had to go to bed.
Next day she pulled it out of the freezer, very thick syrup like substance and the hydroquinone was very visible. Before she did the acid wash she ran it through several coffee filters.
Then it was dumped into a 4L sep funnel along with the 1.5L slightly acidic water. Then it was shaken to mix but the entire sep funnel then turned black from the hydroquinone sticking it the inner surface she presumes. She then shook the sep funnel vigorously and it helped clear it up to determine the layers. Let sit for 20 minutes. She then could see the upper water layer, then also the oraganic lower layer. Lower layer was black, and the top layer a light blood red watery substance. So she assumed to drain off the black layer and leave the upper water layer. When she tried to drain it clogged with the hydroquinone. So she then ran it all through more coffee filters until it was able to drain off. then the upper water layer was washed with first 100ml DCM wash. She could see the oil falling right out of the water into the bottom. it was a light red clear oil. She did this 3 times for a total of 3X100 ml dcm washes. Then all the washes were added together and washed twice with 2X150ml NaOH. That pulled all the remaining hydroquinone out, it was very visible the dark crap went to the top, and the oil fell to the bottom. The upper dark crap layers were tossed.
Then after all that she had almost a full 500ml flask full of this red blood like substance. She set up for vac distillation but the DCM kept jumping to the receiving flask so she distilled off the dcm without vac. all the dcm came over at around 50-60 degrees. There seemed to be about 200-300 ml dcm. Then she turned the vac on. And more substance started coming over at around 100 degrees. Then when it hit 140 degrees she removed the receiving flask and dumped it into a jar. Now this fraction was light red pink. then there was about 30 gram left of this dark dark red with a hint of green substance. Now nothing is distilling anymore and her ghetto hot plate setup is a bitch to regulate (hot plate/stirrer with tin foil tent). the temp now is climbing up and hits 170 degrees and she could see vapors but the temp blasted up to 180 degrees so she pulled it apart and killed the vac worried she would destroy the ketone at that temp. She also noticed a few drops were in the receiving flask and they had a hint of green.
After all this she weighed the distilling flask and realized there was only 30 grams of liquid. That does not correlate with brightstars 100 gram ketone. So she chalked this up to a FAIL.
Now she isnt giving up but needs help. Next step is buying a good heating mantle with good temp control and magnetic stirrer.
Also a note when she distilled the sassy oil, between 100-140 degrees oil was coming over. She is now thinking her safrole isnt pure? Want to test it but hard finding conc. sulfuric acid.