3,6-Dihydro-3-methyl-N-nitro-2H-1,3,5-oxadiazin-4-amine synthesis
- Product Name:3,6-Dihydro-3-methyl-N-nitro-2H-1,3,5-oxadiazin-4-amine
- CAS Number:153719-38-1
- Molecular formula:C4H8N4O3
- Molecular Weight:160.13
Yield:153719-38-1 71.5%
Reaction Conditions:
with acetic acid at 70; for 6 h;Large scale;
Steps:
1 Preparation of 3,6-dihydro-3-methyl-N-nitro-2H-1,3,5,oxadiazin-4-amine
100 kg of N-methyl-nitroguanidine and 64kg of Paraformaldehyde were charged to a 1 000L reactor. 350 kg of acetic acid were added, after which the resulting mixture was heated to 70°C and held at this temperature for 6 hours. Thereafter, the solvent (acetic acid) was removed by distillation under vacuum. 175 kg of 10% NaOH aqueous solution was added with stirring, after which theresulting mixture was cooled and stirred for 30 minutes. The resulting mixture was discharged into a centrifuge for separation. The resulting cake was dried using a Biconical dryer, yielding 98 kg of 3-methyl-N-nitro-1 ,3,5,oxadiazinan-4-imine as white powder (purity 97%, yield 71 .5%).
References:
ROTAM AGROCHEM INTERNATIONAL COMPANY LIMITED;BRISTOW, James Timothy WO2015/180585, 2015, A1 Location in patent:Page/Page column 10; 11
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