.jpg "Research Chemical Sciences")
Jake
Active member
More fun for the chemists. Very close to the original discovery of test base.
4AD to test base
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY
#75 (1953)
page 5930
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:
beakers
hotplate with built in stirrer
stirring bars
distilled water
methanol
chloroform (can be cheaper grade)
thermometer (-10 to 150 degrees celcius, its like $4)
4AD powder
activated MnO2 (if this cannot be found, make your own from potassium permanganate and manganese sulfate. also need ether if you do this step)
filter paper
funnel (holds filter paper)
erlmeyer flask with vacuum tube out side for vacuum filtering
scale
Note-Today you can buy Mn02.
HOW TO MAKE MnO2:
Take concentrated aqueous potassium permanganate and add to a stirred aqueous manganese sulfate solution kept at 90 degrees celsius (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 celsius for 15 minutes. filter, wash well with hot water, then methanol and ether. dry at 120 to 130 degrees celsius 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.
METHOD:
Once the manganese dioxide is made, 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 crystalise 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. 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...Note- don't forget to discard the powder properly as this is an experiment!!
This is not a step by step cookbook recipe. Why? So that only a chemist will be able to follow.
THIS SHOULD WORK JUST THE SAME FOR 19nor4diol to NANDROLONE
4AD to test base
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY
#75 (1953)
page 5930
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:
beakers
hotplate with built in stirrer
stirring bars
distilled water
methanol
chloroform (can be cheaper grade)
thermometer (-10 to 150 degrees celcius, its like $4)
4AD powder
activated MnO2 (if this cannot be found, make your own from potassium permanganate and manganese sulfate. also need ether if you do this step)
filter paper
funnel (holds filter paper)
erlmeyer flask with vacuum tube out side for vacuum filtering
scale
Note-Today you can buy Mn02.
HOW TO MAKE MnO2:
Take concentrated aqueous potassium permanganate and add to a stirred aqueous manganese sulfate solution kept at 90 degrees celsius (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 celsius for 15 minutes. filter, wash well with hot water, then methanol and ether. dry at 120 to 130 degrees celsius 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.
METHOD:
Once the manganese dioxide is made, 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 crystalise 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. 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...Note- don't forget to discard the powder properly as this is an experiment!!
This is not a step by step cookbook recipe. Why? So that only a chemist will be able to follow.
THIS SHOULD WORK JUST THE SAME FOR 19nor4diol to NANDROLONE
