反应详情

The solution of 2-nitro-2-aza-1-propanol in methylene chloride produced in Example 2 was combined with an additional 56 grams of methylnitramine. This mixture was slowly added to 300 ml of stirred concentrated sulfuric acid which had previously been cooled to -5° C. to -10° C. The temperature of the reaction mixture was kept at from 0° C. to -5° C. throughout the controlled addition. After the addition was completed, the mixture was poured into a large excess of ice water. Following the separation of the methylene chloride phase, the water phase was repeatedly extracted with methylene chloride. All the methylene chloride fractions were then combined, twice washed with water, and then dried with magnesium sulfate. The magnesium sulfate was filtered out and then the methylene chloride was removed by evaporation under vacuum, leaving an oily liquid. The oily liquid was converted into solid white crystals of 2,4-dinitro-2,4-diazapentane (m.p. 56° C., 65 grams pure) by precipitation from a chloroform/hexane solvent mixture.

1. additionThis mixture was slowly added to 300 ml
2. temperaturehad previously been cooled to -5° C. to -10° C
3. additionThe temperature of the reaction mixture was kept at from 0° C. to -5° C. throughout the controlled addition
4. additionAfter the addition
5. customthe separation of the methylene chloride phase
6. extractionthe water phase was repeatedly extracted with methylene chloride
7. washtwice washed with water
8. dry with materialdried with magnesium sulfate
9. filtrationThe magnesium sulfate was filtered out
10. customthe methylene chloride was removed by evaporation under vacuum
11. customleaving an oily liquid
12. customThe oily liquid was converted into solid white crystals of 2,4-dinitro-2,4-diazapentane (m.p. 56° C., 65 grams pure) by precipitation from a chloroform/hexane solvent mixture