metanoid - 7-8-2006 at 07:51
Hi!
i'm foreign, so apriori sorry for my language
Its actually intresting for me,
does somebody know practical value of 2 methodics for preparation Bz-Cl from Bz-OH.
They are:
1) 1M BzOH + 1,5M Na2SO4 unhydrous + 1,1M HCl gas (calculating by mass difference) then stirring for approx 3 hrs decantation and distillation
2) 2M ZnCl2 + 2M HCl conc + 1M BzOH then refluxing for 3 hrs. After that upper layer is decantated and boiled with equal volume H2SO4 for 30 min and
simple distillation.
Thanks for attention,
good day
evil_lurker - 7-8-2006 at 08:46
BzOH is easily chlorinated... in my experience no ZnCl or H2SO4 needed.
Use common 10 molar HCl.
3 moles BzOH + 1-3 moles HCl (aq)
Heat in 90-100C water bath, gas with HCl until no more gas is absorbed. Stir for a couple hours afterwards, then separate and distill under
atmospheric conditions.
metanoid - 7-8-2006 at 08:54
thnks
very attractive
i'll try this procedure this night!
jack-sparrow - 8-8-2006 at 07:35
Very simple, put your Bz-OH in a separation funnel along with 20 volumes of HCl 37%, shake and let decant over couple days( forms an emulsion).
Decant, wash with water, bicarbonate, water and brine. Dry MgSO4 and short path distill.