edo (Stranger)
04-16-04 05:30
No 501032
       basifying with NaOH instead of KOH     

Swim is doing Osmium/BrightStar Reductive Amination (../rhodium /redamin.os-bs.html).

 Swim wants to substitute 230g KOH with NaOH.

 How much(grams) of NaOH does swim need to use?Post 234266 (grayIC: "NaOH versus KOH and others newbie questions.", Newbee Forum)
THanks.  smile 		 
 
 
 
    ApprenticeCook
(Hive Bee)
04-16-04 09:07
No 501052
       use the mol.w and work it out...     

use the mol.w and work it out... if you dont know how its a bit strange your doing any chem proceedures at all.

Here it is...
mw(KOH) = 39.1+1.008+16 = 56.108
mol(KOH) = 230/56.108 = 4.099
mw(NaOH) = 22.99+1.008+16 = 39.998
mass(NaOH) = 4.099*39.998 = 163.95g

You need 163.95g of NaOH. Good luck.
-AC 		 
 
 
 
    edo
(Stranger)
04-16-04 11:19
No 501063
       Thanks for calculations. :-)     

Thanks for calculations.



smile 		 
 
 
 
    edo
(Stranger)
04-17-04 02:20
No 501154
       concentration of acid     

Swim just bought sulfuric acid from local auto store. After looking at the MSDS sheet it only contains 10% H2SO4 http://www.jtbaker.com/msds/englishhtml/s8236.htm

In LoBtops write up Post 208821 (LaBTop: "The ONE and ONLY buffered Performic", Methods Discourse)he uses 15%  H2SO4.

Is 10% ok?

Thanks 		 
 
 
 
    Rhodium
(Chief Bee)
04-17-04 02:23
No 501156
       should work     

It should work, just let it react for a little longer, say 3.5 hrs.
The Hive - Clandestine Chemists Without Borders 		 
 
 
 
    ephemeral
(Stranger)
04-17-04 03:04
No 501176
       H2SO4 vs. HCL for glycol hydrolysis     

referencing  Chromics HCL post  (476334) and V. Verdsegast there as well concerning HCL in place of sulfuric,  they used an alcohol solvent with the glycol, then H2O with the HCL.
      The question is, what ratio of  alcohol/water/acid is appropritate? That is, how is the amount of solvent determined in each case, a molar ratio?  But when scaling up, is it correct to increse the solvent quantity accordingly, or use a lessor amount?
  Thanks for any reference 		 
 
 
 
    edo
(Stranger)
04-17-04 04:10
No 501188
       Thanks Chief Bee! :-) For some reason swim...     

Thanks Chief Bee!smile

For some reason swim thought H2O2 otc was 35%(but it only 3%).  Swim mixed the 3% H2O2 with formic acid and dripped 1/2 of solution into iso,baking soda,dcm before he realized his mistake.  Yea swim is an idiot shocked

What should swim do?
Swim will be picking up 35% H2O2 soon from local chem shop.
for now can swim take 3% H2O2 and boil off water to concentrate the H2O2 until 35% is achieved
Can iso,Na2CO3,dcm mixture be saved?

Plz advise
xia xiasmile 		 
 
 
 
    ephemeral
(Stranger)
04-27-04 04:14
No 503235
       Sorry to be repetative, but could someone give     

Sorry to be repetative, but could someone give advice on the proper ratio of  HCL/alcohol/glycol  when unsing HCL for a glycol hydrolysis  in a performic rxn?

   TFSE is still closed and cant find this info.  Also, is standard  muriatic equivlent to 5 normal? ie  15%  ?

 thanks muchsmile 		 
 
 
 
    amine
(Hive Bee)
04-27-04 04:48
No 503243
       The ratio....     

2g glycol : 3ml MeOH : 5ml dH2o : 5ml 31.25% HCL

so a nice 2:3:5:5 ratio :).

Reflux for 2.5hr.

The temp of the solution should stay around 86C during the reflux.

Scale up as your see fit. (Swim did a nice scale up on 200g of glycol..all went well) (this are Chromic's specs adjusted  a little bit) 		 
 
 
 
    ephemeral
(Stranger)
04-29-04 04:35
No 503659
       My sincere thanks Amine!     

My sincere thanks Amine!smile  Coulnd't seem to properly extrapolate this info, and this was likely one of the errors in SWIMs earlier runs.  Will apply and report results.
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