explodes at 300 °C
MEDINA stands for methylene dinitramine, and is also called methylenedinitramine and N,N-dinitromethanediamine. This compound was first prepared around 1949 at the University of Bristol by the hydrolysis of hexamine. This compound is not cruelty free (heh heh), it has been sprayed into rabbit eyes and injected under guinea pigs skins. The compound has been found to be non-toxic. This lab does not exactly fit in well with normal laboratory procedures as this information is the industrial laboratory method. Since this is the industrial method and it is still made in the lab I conclude this substance is either not used much or is to dangerous, I am leaning towards not used much. This is surprising as this explosive is quite powerful for such a small and simple molecule. Its real fault lies in the fact that it does not keep well, so use it soon after preparing.
|acetic anhydride||50 & 250-mL beaker|
|charcoal||2-L Florence flask|
|ethyl acetate||graduated cylinder|
|ethyl alcohol||stirrer/stirring rod|
This is a three step process for the manufacture of MEDINA: In a round bottom 2-L Florence flask, mix 476 mL of formamide and 70 g of methenamine. The flask is set up for refluxing, and heated at 140 °C for 5 hours. It is then chilled in ice, the solid is filtered, and washed on a filter with 90 g of formamide. The crude product of methylenediformamide may be used in the next step or purified by dissolving in ethyl alcohol, decolorizing with charcoal, and chilling.
19 mL of 100% nitric acid is added dropwise with a buret while stirring to a suspension of 5 g of crude methylenediformamide in 19 mL of acetic anhydride cooled to 10-15 °C in a 50-mL beaker. The solution is then held at 0 °C for 2 hours, and poured with stirring into a 250-mL beaker filled with 150 mL of ice water. The precipitate is filtered, washed twice by mixing with ice water, pressed dry on the filter, and dissolved in 30 mL of ethyl acetate. The solution is seperated from water, dried over anhydrous sodium sulfate, concentrated in vacuum, 10 mL of isopropyl alcohol is added, and the product is collected. The product is methylene di(nitroformamide), which can be purified by recrystallization from either acetone, isopropyl alcohol, or from boiling ethyl chloride.
The crude methylene di(nitroformamide) is pressed dry on the filter, stirred into 105 mL of formic acid, and the paste is allowed to stand overnight. The next day the solution is filtered through an acid filter, the formic acid and water is removed by distilling with xylene, and the crude MEDINA, which seperates as a sand, is filtered and dried over paraffin and sodium hydroxide in vacuum. The crude MEDINA is recrystallized from 2-nitropropane or a 9:1 solution of ethyl chloride/isopropyl alcohol. You will need a graduated cylinder for measuring liquids, a stirring rod or magnetic stirrer for mixing, and a thermometer to monitor the temperature.
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