delta_acrylate
August 25th, 2004, 06:43 PM
The compound 3,4-diaminofurazan is an explosive precursor for the synthesis of several explosives, for example:
Synthesis of 3,3'-diamino-4,4'-azoxyfurazan (DAAF).
To 100 g of hydrogen peroxide maintained at 18°C, add 55 g of sulfuric acid over 10 min with stirring. Than add 10 g of 3,4-diaminofurazan. The suspension is stirred for 24 hrs and the green soluble nitroso-aminofurazan is converted to the insoluble orange DAAF.
Theorical Yield: 88%
Synthesis of 3,3'-diamino-4,4'-hydrazofurazan.
Charge in 1 Lt Erlenmeyer flask 200 ml of methanol, 10.6 g of DAAF and 9.77 g of Zn dust. To this suspension add 9 g of acetic acid dropwise over 10 min. with good stirring. The slurry is stirred for 1 hr and filtered through a bed of celite. The bed is washed with methanol and the solvent removed under reduced pressure.
Theorical Yield: 100%
Synthesys of 3,3'-diamino-4,4'-azofurazan (DAAzF).
Air is bubbled through the methanol solution of the hydrazo-furazan, for 20 hrs with stirring at room temperature. The orange precipitate is filtered and washed with methanol and air dried.
Synthesis of 1,4,5,8-tetranitro-1,4,5,8-tetraazadifurazano-[3,4-c][3,4-h]decalin.
Part 1 1,4,5,8-tetraazadifurazano-[3,4-c][3,4-h]
A 10 g portion of 3,4-diaminofurazan is added to a solution of 10 g 37% HCl in 20ml of distilled water. This slurry is stirred at 60°C while 7.25 g of 40% aqueous gluoxal is added. The mixture is stirred for one additional hour and then cooled. The product is collected and washed well with water.
Theorical Yield: 98%
Part 2 Nitration of 1,4,5,8-tetraazadifurazano-[3,4-c][3,4-h]
In a 100 ml r.b flask a magnetic stirring bar and 14 ml of trifluoroacetic anhydride are placed. After cooling to -5°C in a salt/ice bath, 6.0 ml of 100% HNO3 is added dropwise, with stirring over a period of 20 min. This mixture is allowed to warm briefly to room temperature. Then is was recooled and 2.22 g of 1,4,5,8-tetraazadifurazano-[3,4-c][3,4-h] is added in small portions over a period of 10 min. The mixture is allowed to slowly come to room temperature over a period of 4 hrs.. The product is collected by vacuum filtration under a blanket of N2 and washed well with methylene chloride, The last traces of solvent a removed under vacuum.
For more information on this procedures refer to US Pat 6358339 and 4503229
Sounds easy to make, but i cant find any synthesis for 3,4-diaminofurazan, i hope that anyone in the forum has a procedure for the synthesis of this explosive precursor.
Synthesis of 3,3'-diamino-4,4'-azoxyfurazan (DAAF).
To 100 g of hydrogen peroxide maintained at 18°C, add 55 g of sulfuric acid over 10 min with stirring. Than add 10 g of 3,4-diaminofurazan. The suspension is stirred for 24 hrs and the green soluble nitroso-aminofurazan is converted to the insoluble orange DAAF.
Theorical Yield: 88%
Synthesis of 3,3'-diamino-4,4'-hydrazofurazan.
Charge in 1 Lt Erlenmeyer flask 200 ml of methanol, 10.6 g of DAAF and 9.77 g of Zn dust. To this suspension add 9 g of acetic acid dropwise over 10 min. with good stirring. The slurry is stirred for 1 hr and filtered through a bed of celite. The bed is washed with methanol and the solvent removed under reduced pressure.
Theorical Yield: 100%
Synthesys of 3,3'-diamino-4,4'-azofurazan (DAAzF).
Air is bubbled through the methanol solution of the hydrazo-furazan, for 20 hrs with stirring at room temperature. The orange precipitate is filtered and washed with methanol and air dried.
Synthesis of 1,4,5,8-tetranitro-1,4,5,8-tetraazadifurazano-[3,4-c][3,4-h]decalin.
Part 1 1,4,5,8-tetraazadifurazano-[3,4-c][3,4-h]
A 10 g portion of 3,4-diaminofurazan is added to a solution of 10 g 37% HCl in 20ml of distilled water. This slurry is stirred at 60°C while 7.25 g of 40% aqueous gluoxal is added. The mixture is stirred for one additional hour and then cooled. The product is collected and washed well with water.
Theorical Yield: 98%
Part 2 Nitration of 1,4,5,8-tetraazadifurazano-[3,4-c][3,4-h]
In a 100 ml r.b flask a magnetic stirring bar and 14 ml of trifluoroacetic anhydride are placed. After cooling to -5°C in a salt/ice bath, 6.0 ml of 100% HNO3 is added dropwise, with stirring over a period of 20 min. This mixture is allowed to warm briefly to room temperature. Then is was recooled and 2.22 g of 1,4,5,8-tetraazadifurazano-[3,4-c][3,4-h] is added in small portions over a period of 10 min. The mixture is allowed to slowly come to room temperature over a period of 4 hrs.. The product is collected by vacuum filtration under a blanket of N2 and washed well with methylene chloride, The last traces of solvent a removed under vacuum.
For more information on this procedures refer to US Pat 6358339 and 4503229
Sounds easy to make, but i cant find any synthesis for 3,4-diaminofurazan, i hope that anyone in the forum has a procedure for the synthesis of this explosive precursor.