obituary (Hive Addict)
07-29-01 21:08
No 199920
      synth of phloroglucinol  Bookmark   

from org synth IX 

225g (0.87mol) of crude 2,4,6-trinitrobenzoic acid is placed in 1800ml of conc HCl in a 5L flask witha  reflux condensor.  add to this 825g (7mol) granulated Sn in small portions - the rxn starts after about 30-40g of tin added and then placing on a hot water bath.  add the rest through the condensor to keep a good reflux and reaction rate going.  after completion of the addition- heat on steam bath for another hour.  then filter to remove the unreacted Sn. 

neutralize with NaOH solution. keep in mind your titrating the Sn with acid also. should take about 800ml of a 40% NaOH sol.  dilute the mix to 6L and place in a 12L flask.  boil at reflux in an inert atmosphere (coal gas, CO2, N2, argon, H2 will all work)  for 24 hrs.  filter the precip and wash with about 2-3L of boiling H2O.  add HCl til just acid to litmus and chill to 0*C.  filter.  should be around 70-80g phloroglucinol. dissolve in 700ml of hot water filter and cool to 0*C and filter off and keep these crystals 65-75g of phloroglucinol----46-53% yeild.
MP 217-218*C

1,3,5-trinitrobenzene can be sub'd for the tri-nitro acid, but the acid is usually cheaper. 

phloroglucinol is also made by :

NaOH fusion with maclurin or kino (vegatable products)
NaOH fusion with Phenol or better yet with resorcinol
fusing 1,3,5-benzene trisulfonic acid w/NaOH
fusing 3,5-dibromophenol with KOH
best yeilds from boiling triaminobenzene HCl or triaminobenzoic acid HCl with H2O

ref's for the other rxns can be given if requested.
(Stoni's sexual toy)
07-30-01 01:07
No 199970
      Re: synth of phloroglucinol  Bookmark   

If I had a source for TNT I think I wouldn´t convert that to trinitrobenzoic acid wink

But a nice find anyway. Drug precursor from explosives. Interesting.
(Hive Addict)
07-30-01 14:49
No 200112
      Re: synth of phloroglucinol  Bookmark   

TNT's actually really easy to make though.
(Stoni's sexual toy)
07-30-01 14:51
No 200113
      Re: synth of phloroglucinol  Bookmark   

Sure, because oleum can be found in every hardware store.