Hello good folks out there in the Hive, I am new to the Hive and, after extensive reading and research, am about to embark on my first synthesis. I am hoping I can get some feedback on a synthesis from RHODIUM’S site entitled “MDP2P FROM SAFROLE USING H2SO4 AND NH4NO3” which entails the following procedure:
Collect clean Safrole and chill to 0 c. in a freezer.
Prepare 80% H2SO4 and also chill to 0.c in freezer.
Add 20g. CHILLED Safrole to 250ml. R.B.F, placed upon stirrer in ice/salt bath (-5.C).
Place CHILLED 80% H2SO4 in CHILLED drop funnel and add to Safrole at 3 drops per second.
After this addition, put 80ml. CHILLED DH20 in drop funnel and add to H2SO4/ALKENE at 3-4 drops per second.
When finished place contents of 250ml. R.B.F. into sep. funnel, add salt, discard lower portion, dry over MG2SO4, to reveal 20-22 g. of MDP2Pol.
Combine 20g. MDP2Pol to 20g. NH4SO3 and CHILL, in a R.B.F, in an ice bath, add 30 ml. G.A.A., a “dash” of CUPRIC ACETATE and 5 ml. DH2O.
Gently heat for 10-15 mins, cool mixture, filter, separate RAW MDP2P layer from liquid portion via 3x D.C.M., combine extracts, dry over MG2SO4 and evaporate D.C.M. to yield 20g. red/yellow oil.
Filter through SILICA/BUCHNER to yield 19-20g. MDP2P.
The write-up is incoherent and there is also a disclaimer questioning the validity of this process, so could anyone please let me know:
Does this process, in fact, work? And if so
Have I interpreted it correctly?
Can store bought AMMONIUM NITRATE be used?
If it has any additives will this affect this process?
Could dry ice be used in the cooling process or will this be too cold and freeze the DH2O/G.A.A. content?
If this works I am considering a LEUCKHART REACTION to convert my KETONE. The synthesis, also from the excellent RHODIUM site is listed below, I would appreciate any comments on this also (e.g. Is there a way I can get a better yield with my leuckhart than the proposed 70%). It goes as follows:
Add 4 parts KETONE, 11 parts FORMAMIDE, 0.2 parts G.A.A and 2 parts DH20 to a suitably sized distillation set-up with the thermometer reaching into the mix.
Heat oil-bath to 100. C and SLOWLY raise to 150.c to keep reaction moving along.
Let reaction cool, add vacuum Adapter and distill off FORMAMIDE under vacuum.
Add 60 g. KOH to 160 ml. ETHANOL and 50 ml. DH20 to leftover residue and reflux for 20 mins.
Evaporate ETHANOL, filter over SILICA/BUCHNER, basify with 25% NAOH, extract with 3x D.C.M., combine extracts and dry over MG2SO4.
Yield is said to be 70%
Crystallize by SLOWLY dripping 100% I.P.A./H.C.L. to D.C.M/ M.D.A. and filter to collect crystals. Enjoy.
If these processes are both viable one could make up a beautiful batch of MDA/HCL in a few hours.
THANKS,
PIHKALS & ICECREAM