JOURNAL OF THE AMERICAN CHEMICAL SOCIETY
sondheimer et al.
1g 4AD + 100mL chloroform + 10g MnO2 = test base 100% after 2 hours shaking at room temp
yield is 93% when crystalized with methanol and filtered on paper
MATERIALS: (check www.sciencelab.com
i don't know if they are the cheapest, but they have everything)
hotplate with built in stirrer
chloroform (can be cheaper grade)
thermometer (-10 to 150 degrees celcius, its like $4)
activated MnO2 (if this cannot be found, make your own from potassium permanganate and manganese sulfate. also need ether if you do this step)
funnel (holds filter paper)
earlmeyer flask with vacuum tube out side for vacuum filtering
now that is alot of MnO2 and it can be done with less. too simple you say, well your right its not that easy. the MnO2 available commercially is not always active. but the authors gave a method of preparing MnO2 that is easy and the product is very active and can be put in a stoppered jar with no loss of activity (those guys would make great homebrewers)
HOW TO MAKE MnO2:
take concentrated aqueous potassium permanganate and add to a stirred aqueous manganese sulfate solution kept at 90 degrees celcius (need a hot plate that has stirrer built in) until a slight excess was present (pink coloration of the supernatant liquid). stir at 90 degrees celcius for 15 minutes. filter, wash well with hot water, then methanol and ether. dry at 120 to 130 degrees celcius to a constant weight. it can be kept for several months in a well stoppered bottle with no loss of activity.
how to get concentrated aqueous potassium permanganate: take distilled water and and add potassium permanganate until not more goes into solution (this is where a magnetic stirrer comes in handy). if you added too much, just add more water until all is in solution. duh!
how to get aqueous manganese sulfate: same idea as above.
i am looking for a source of activated manganes dioxide so that the above does not need to be performed. once we get the manganes dioxide, all we have to do is mix the 4AD, MnO2 and chloroform in the ratios above, basically add the 4AD to chloroform on the magnetic stirrer and then add the MnO2 and leave it for 3 hours at room temp. add methanol to the solution and the test will crystalize and fall out of solution. filter and wash well with methanol. collect the filtrate and filter again on new filter paper and dry all the filter papers. if the filtrate still has crystals, filter with another paper. i would dry the first filter paper out well for a few days and weigh it. if its more than 80% yield, i wouldn't waste time trying to get the rest. if not, then take the filtrate and refilter to get rest of crystals. you kind of play it by ear. that's pretty much it.....oh yeah, don't forget to discard the powder properly as this is an experiment
it is possible that much less MnO2 can be used. this will mean that the reaction will have to sit longer maybe a day or two, i don't really know. this will have to be found out. i want to try this in the lab where i can measure the ultraviolet spectrum to determine how long the complete reaction takes with different amounts of MnO2 and chloroform so as to minimize cost.
why did i not do it step by step? well if you can't figure it out, then you probably shouldn't be doing it.
THIS SHOULD WORK JUST THE SAME FOR 19nor4diol to NANDROLONE
ba-doop, ba-doop, that's all folks