Krypton
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Location: Spain
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Easy Synthesis of MEDINA ?
Dry out the synthesis of MEDINA from dichloromethane and ammonia.
To 25% ammonia solution add sodium acetate to bound the chlorine and than add dichloromethane and stirr at room temperature for 2 hours. Than boil out
the ammonia at 50 C and and than cool to 5 C and add concentrated HNO3 dropwise and than concentrated H2SO4.
Keep the temperature below 5C.
Filter out the white sand and and dissolve in 3 times in destilled water and evaporate the ater at 60 C.
I don`t know if the synthesis work well ?
You must dry out the amonts self.
In convention with my ancestor.
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KABOOOM(pyrojustforfun)
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diaminomethane is condensation product of formaldehyde and ammonia whether it is made from it or not! such compounds in aqueous solutions are
equilibrating with the corresponding aldehyde and ammonia acidic environment leads the reaction to the right side
CH<sub>2</sub>(NH<sub>2</sub> <sub>2</sub> +
H<sub>2</sub>O <s><sub><</sub>___></s> HOCH<sub>2</sub>NH<sub>2</sub> +
NH<sub>3</sub>
HOCH<sub>2</sub>NH<sub>2</sub> + H<sub>2</sub>O <s><sub><</sub>___></s>
HOCH<sub>2</sub>OH + NH<sub>3</sub>
HOCH<sub>2</sub>OH <s><sub><</sub>___></s> CH<sub>2</sub>O + H<sub>2</sub>O
sulfuric acid probably destroys MEDINA (like most other nitramines)
what is the role of sodium acetate there? keep the PH ideal for the first reaction?
anyone tried to nitrate the methylene diamide with H<sub>2</sub>SO<sub>4</sub>-HNO<sub>3</sub> ? (standard methods
use Ac<sub>2</sub>O-HNO<sub>3</sub>
<b>another method</b>
nitrosoation of methylene diamide (in aqueous sol of course) should yield the di(N-nitroso<i>alkylamido</i>methane crystals. it needs to be oxidized (I'm seekin for your opinions guys!)
then hydrolyzed.
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Anders Hoveland
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Preparation of precursor: Methylenedinitroformamide:
In a 1 liter reaction vessel place-A mixture of 70 grams of hexamine(0.5mole) and 270 grams(6mole) of freshly distilled formamide were heated to 140
deg C and maintained for 4 hours.
On cooling the crystals were separated.
Initial yield is 87.8 grams(29% of theory)
To obtain more crop,the mother liquor was retained and to it was added 23.5 grams of hexamine and 90 grams of formamide.Heat the mixture to 140deg C
for 5 hours.Cool the mixture and separate the resulting crystals.
Succeeding yields range from varies from 80-100 grams per reaction run.
If you desire to obtain more precursor,Repeat this procedure for 8 times using similar quantities hexamine and formamide(23.5grams & 90 grams
respectively).This will takes about 50 hours consuming totally 281.5 grams of hexamine and 1080 grams of formamide.The total yield of
methylenediformamide is 1034 grams(nearly 78%of theory).
Reaction equation
(CH2)6N4 + 12 HCONH2 -----> 6H2NC=O-CH2-C=O-NH2
The pure product is a white crystalline material melting at 140-141degC.It is soluble in water at an extent of 100 grams per 100 cc.and 6.6 gram per
100 cc of isopropanol.
Preparation of Methylenedinitramine:
Place the 2-3 liter reaction vessel preferably in a dry ice-kerosene bath so as to much better control the temperature of the exothermic reaction
between nitric acid,acetic anhydride and methylenediformamide.
Nine moles( 380 grams) of 100% HNO3 was added as rapidly as possible at +-2deg C. to a well stirred suspension of 102 grams (1 mole) of
methylenediformamide in a 380 ml(4 mole) of acetic anhydride.
Upon completion of the nitric acid addition,remove the dry ice-kerosene bath,and replace it with an ice-bath.Allow the reaction to age over this ice
bath for 4 hours.
You will notice that after the application of the ice -bath,the temperature of the reaction will rise to 8deg C for 15-30 minutes and then fell to
+2deg C where it remained during the aging period.
At the end of the aging period the reaction mixture was poured slowly with stirring into a mixture of one liter water and 1000-1500 grams of cracked
ice.
The methylenedi(nitroformamide) was immediately collected on a filter and washed with three 100 ml portions of ice –water.The filter cake was
pressed with a rubber dam.The yield at this point was 190-220 grams of damp material.
This methylenedi(nitroformamide) is stirred into 100 ml of formic acid and the resulting paste allowed to stand overnight.
The following day the mixture was warmed to 65 deg C to dissolve the methylenedinitramine which has crystallized. Filter and cool to ice
temperature(and seed it preferably to cause crystallization.One way of doing this is to rub gently the end of the stirring rod inside the walls under
the crystallizing solution).This crystallization will take 5-6 hours.The crystals were collected on a filter and washed with benzene (or toluene).
The yield at this point is 70-80 grams of pure methylenedinitramine(50-60% based on methylenediformamide.
To obtain a second crop of methylenedinitramine,the mother liquor(with formic acid) was concentrated under reduced pressure and cooled to ice
temperature and seeded to cause crystallization.The calculated total yield was 75-85% of theoretical based on the amount of methylenediformamide,about
100-115 grams of MEDINA.
Reaction equation
Formation of methylenedi(nitroformamide).
H2NC=O-CH2-C=ONH2 + (CH3CO)2O + 2HNO3--> H2N-NO2-CHO-CH2-CHO-H2N-NO2 + CH3COOH
Hydrolysis with formic acid
H2N-NO2-CHO-CH2-CHO-H2N-NO2 + H2O ( in HCOOH)-->HNNO2-CH2-NNO2H
For further purifications of Methylenedinitramine.Recrystallize it from a 9/1 by volume mixture of either of these solvents composition:
ethylenedichloride/isopropanol,
ethylenedichloride/2-nitropropane
ethylenedichloride/95%acetic acid
The purified Methylenedinitramine melts at 105-106deg C.It begins to decompose with the evolution of gas at 110degC.
this was found at explosive and weapons forum
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Reference
Anders Hoveland
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Registered: 12-7-2010
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Has anyone made mixed hydrazine with MEDINA?
Would this ionic compound be denser or maybe harder to detonate?
MEDINA is acidic and when neutralized by a base, it becomes more stable, but forgive that I cannot find a reference. I swear I read this somewhere.
A +2 ion and a -2 charged ion pack into dense, more poorly soluble crystals, usually.
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Reference
Anders Hoveland
Posts: 13
Registered: 12-7-2010
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Quote: Originally posted by KABOOOM(pyrojustforfun)  |
nitrosoation of methylene diamide (in aqueous sol of course) should yield the di(N-nitroso<i>alkylamido</i>methane crystals. it needs to be oxidized (I'm seekin for your opinions guys!) then
hydrolyzed. |
In another thread, it was (sort of) established that primary nitrosamines are not stable. If methylene diamide can exist in solution, a much simpler
method may be to dissolve hexamine in ammonium hydroxide. But there is really no need to make it, since all sorts of combinations are in equilibrium
when hexamine begins to disintegrate as the pH goes down.
I am sure there could be a synthesis that can start with hexamine to make MEDINA
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