many of you have seen my other posts about making steroids synthetically but always in the context of a laboratory setting, a masters in organic synthesis etc.. Lord knows over the years i have had my hands in a fair number of batches of a multitude of steroids, many of you have probably tasted my fruits but will never know.
myself and the boogeyman set out to attempt to do this synthesis with absolutely nothing from a scientific supply house, no glassware, no ph papers no all. We succeeded and ended up with base test so pure it crystallized like shattered glass.
THEORY: DHEA is two synthesis steps away from test base, one oxidation, one reduction. The most logical way is to reduce first the 17=O to create 5 androstenediol, this way there are many selective oxidation agents that will only convert the 3-OH to a =O and not the 17. Since DHEA is not water soluble one can not use water as a solvent for the reaction, the obvious choice is methanol since the reduction is done with sodium borohydride. A large excess of methanol is used because 5androdiol is much less soluble in methanol than DHEA so as it is formed it will slurry. The second step is full of possibilities but the available selective oxidizer is manganese dioxide, in this case the reaction is done in acetic acid which gives slight solubility to the androdiol to transiently come in and out of solution to react
experimental: DHEA was purchased from china in one kg quantity, methanol or methylhydrate from canadian tire, sodium borohydride from a hydrogen cell engine supplier online fifteen grams for fifteen dollars, good for 60 grams test. 10 grams DHEA dissolved in 400ml methanol and stirred using a milk frother in a regular glass nestled in ice. 2.5 grams sodium boro are slowly added as powder at a rate that does not allow the temp to exceed 40C. if a slurry forms thats good, it means product is forming, just add more cold methanol. after a total of one hour add vinegar until the bubbling on addition stops then dump into a liter of ice water. filter thru coffe filter and squeeze dry. dry in oven at 60C.
activated manganese dioxide is made from manganese dioxide from a ceramics supplier and then its boiled in nitirc acid to activate. make nitric acid by adding boiled down battery acid to stump remover (potassium nitrate) then boiling inside a bottle with a hose running to another bottle nestled in ice to collect the nitric acid. filter and rinse with an anhydrous solvent like a fuel system water remover, activated mang diox must be absolute dry. put the diol from the first step in 300ml acetic acid then slowly add the mang diox as a powder same fashion as above, stir for six to ten hours, you won't over oxidize since exact molar equivalents are used. now flood the reaction with five times volume ice water and filter out the base test plus unreacted diol and DHEA, minimum purity will be about 70%
note we activated mang diox by azeotropic distillation with benzene as we are too lazy to make nitric acid.
75 grams of DHEA can be had for about a buck a gram, all together maybe 2-4 dollars a gram for heat free decent test.