Do you want to try this very simple rdxn ?
2.5 gr powdered (coffee grinder) DMNS (put the molar eq.)in 20 methanol and 4 ml HCl 36 %(mix methanol and HCl first and let it cool to room temp), put in a water/ice bath and when it is at 4 C add 0.5 grams of Zn dust, when temp descends to 4 C add 1.5 ml HCl, let cool again and repeat till you have added 12.5 C of Zn and 36 ml of HCl, keep rxn cooling with the ice bath at 4-6 C or less 6 hours (only a bit of Zn will reamin in rxn), let melt and wait 8 hours more. Filter if it remains a bit of undissolved Zn, add 40 ml of water, remove with aspirator methanol, wash with three small portions of DCM (add more water if there's no separation), basify with 40 % NaOH, cooling to not let temp go >30 C (it's better to add acid solution to basic solution, then add more NaOH solution till you have no solids, all hydroxides dissolved), extract with toluene, 3 x 18 % v/v, wash with toluene 1x30 % v/v 40 % NaOH, dry 12 hours with 10 % KOH w/v, filter and wash a bit the KOH with toluene that you will add to the filter, concentrate the toluene and crystallize.
Just follow exactly the instructions, you don't need to be very skilled to make this rxn.
I promise you that you will see dissappear the nitrostyrene in the 5 first additions, and a minimum yield of 50 %, though I believe it will be > 70 %. Same procedure with 2,5 DMNS and only 6.25 gr of Zn dust gave 56 %.
If you try it, please post results. Thanks.
