Well fuck my life I must confess it ain’t as good at all. The yield sucks. Specifically it was 17,7% in SWIM’s case.
SWIM made a rxn w/150 ml water, 70 g of 50% NaMeSO4, 10 g NaOH - to that 9 g HQ in 100 ml water was added in 4 portions over 3 h at reflux (bath temp 140 C, yes that’s how it should bee) – everything under inert atm. 30 min after that time no more oily drops/crystals appeared in the condenser, ~150 ml distillate collected, pure white product filtered out, pressed dry & air-dried, water phase extr’d w/50 ml DCM, dried/evap’d – yielded really negligible amt, ~100 mg of reddish stuff. The weight of the product was 2 g.
SWIM didn’t extract the rxn mixture itself, as he doubts there’s much in it – and it is doomed to bee dirty (the mxtr gets pretty brown at the end)
Well I think it’s not ultimate yet – 1st of all methylsulfate was quite dirty (which SWIM found out only when he got to the rxn – obviously, the Na2CO3 SWIM used to neutralize HMeSO4 contained some washing powder (!!!
I know what you’re thinking of SWIM now – and he deserves it
) And, in addition to that – that methylsulfate contained an unknown quantity of Na2CO3, and, what’s worse, possibly, NaHCO3 (neutralizes NaOH) – so, to summarize all said above, it was again not a scientific experiment
SWIM thinks he’s going to do that one more time – this time
precisely like in the patent (BTW, I noticed they actually used toluene for all extractions! – didn’t specify how they removed it, though)
So there still might bee something similar to a success story yet, although I’m not nearly as optimistic now as I used to bee.
Antoncho