MDA synth and THF alternative?

[Macondor]

-Dont use glacial acetic acid i the reaction like Shulgin in the styrene formation, maybe not need? 3 weeks is a lot of time to do magics things
-The THF can be replace with other solvents?
-Can be used NaBH4 or cyanoNaBH4 for the reduction?
-I see that here for the reaction with LAH not use inert atmosphere like Shulgin, maybe because dont use Heat?

Here is the tarzan RAW synthesis (love it)

"" STEP 1 (Makin' da nitroalkene)

Dissolve 1000 g of piperonal into 500 g of nitroethane containing 66 g of
cyclohexylamine and let the mix stand for about 3 weeks... Then, crush your
'chicken yellow' nitroalkene cake and wash it with about 2 liters of freezer
cold MeOH. Spread to dry...

YIELD: ABOUT 1000 TO 1100 g...

STEP 2 (Reducin' da above mentionned stufff)...

To 200 g of LiAlH4 dissolved in 10 L of ice cold anhydrous THF add dropwise
with cooling, 520 g of raw MDP-2-NP (straight from the previous step)
dissolved in 5 L of THF... The addition should take between 1 to 3 hours with
proper cooling of the reaction mix...

Stir at room temperature for 36 hours... (NO REFLUX!)

Then, add to the mix containing the now reduced compound, 1000 ml of IPA to
decompose the residual LiAlH4... followed by 400 ml of 15% aqueous NaOH...
Filter the solids (Al + Li salts) from the reaction mix and CAREFULLY wash
the filter cake using the remaining 5 L of THF from your 20 L drum...

Evaporate the solvents and crystalize the free base 'à la Shulgin' to get
about 600 g (between 500 to 700 g), of the product HCl.""

 

[Macondor]

"" STEP 1 (Makin' da nitroalkene)

Dissolve 1000 g of piperonal into 500 g of nitroethane containing 66 g of
cyclohexylamine and let the mix stand for about 3 weeks... Then, crush your
'chicken yellow' nitroalkene cake and wash it with about 2 liters of freezer
cold MeOH. Spread to dry...

YIELD: ABOUT 1000 TO 1100 g...

STEP 2 (Reducin' da above mentionned stufff)...

To 200 g of LiAlH4 dissolved in 10 L of ice cold anhydrous THF add dropwise
with cooling, 520 g of raw MDP-2-NP (straight from the previous step)
dissolved in 5 L of THF... The addition should take between 1 to 3 hours with
proper cooling of the reaction mix...

Stir at room temperature for 36 hours... (NO REFLUX!)

Then, add to the mix containing the now reduced compound, 1000 ml of IPA to
decompose the residual LiAlH4... followed by 400 ml of 15% aqueous NaOH...
Filter the solids (Al + Li salts) from the reaction mix and CAREFULLY wash
the filter cake using the remaining 5 L of THF from your 20 L drum...

Evaporate the solvents and crystalize the free base 'à la Shulgin' to get
about 600 g (between 500 to 700 g), of the product HCl.""

-Dont use glacial acetic acid i the reaction like Shulgin in the styrene formation, maybe not need? 3 weeks is a lot of time to do magics things
-The THF can be replace with other solvents?
-Can be used NaBH4 or cyanoNaBH4 for the reduction?
-I see that here for the reaction with LAH not use inert atmosphere like Shulgin, maybe because dont use Heat?

 

[WillD]

You can use the reduction with ordinary amalgam, it will also work good. The use of acetic acid in the first stage is desirable. You can also do the first stage with heating more quickly. Use an excess of nitroethane and recrystallize a product from IPA for more purity.

 

[Macondor]

Thanks for the reply.


-- So in the first stage if i heating for fast reaction is neccesary the use of Acetic acid and use 1 ml of nitroethane for grm of piperanol? like shulgin? , and the cyclohexylamine can stay in 66 grm for 1kg of piperanol?
i need 5 Liter of acetic acid or can i use less? , this raw synthesis is good because i dont need too much reagents, but need patients and time, i am not hurrry je


-- I see that i can replace the THF with Diethyl Ether, there is other solvent that do the job? if the ether have BHT is a problem? or is beter distill the deamon.

-- Ordinary amalgam? what do you mean. Can i replace the LAH with cyanoNaBh4 or NaBH4 ?

-- The inert atmposher for the reduction is neccesary?

thanks again sorry for all the questions