反应详情

A suspension of 0.80g of 1,5-di(trichloroacetyl)-1,3,5,7-tetraazabicyclo[3.3.1.]nonane in 5ml. of liquid dinitrogen tetroxide was stirred in a closed container for 20 hours. The reaction mixture was poured into ice water and the solution was neutralized with potassium carbonate to give a solid precipitate which when recrystallized from nitromethane melted at 234°-235°; yield, 0.41 g. (43%) of 1,5-di(trichloroacetyl)-3,7-dinitrosooctahydrotetrazocine. Upon further treatment of the above precipitate with 4 ml. of 99% nitric acid at room temperature with stirring for 12 minutes, followed by quenching in 250 ml. ice and neutralization with potassium carbonate to a pH of about 8, a yield of 89% of 1,5-di(trichloroacetyl)-3,7-dinitrooctahydrotetrazocine was obtained. The melting point of the product when recrystalized from hot nitromethane was 275°-278° C. and the NMR peak was delta 6.05 (in acetone -d6). The calculated elemental analysis is 19.34% carbon, 1.62% hydrogen and 16.91% nitrogen. The analysis of the product showed 19.22% carbon, 1.56% hydrogen and 16.82% nitrogen.

1. customto give a solid precipitate which when
2. customrecrystallized from nitromethane melted at 234°-235°
3. customyield
4. customby quenching in 250 ml