O.NN.[Cl-:4].[NH4+].[N+:6]([NH:9][C:10]1[NH:11][CH2:12][C:13]([CH3:17])([CH3:16])[CH2:14][N:15]=1)([O-])=O>C(O)CC>[ClH:4].[NH:9]([C:10]1[NH:15][CH2:14][C:13]([CH3:17])([CH3:16])[CH2:12][N:11]=1)[NH2:6]Hydrazine hydrate (1.98 grams; 0.0396 mole) is added to a mixture of 1-propanol (50 mls), ammonium chloride (1.56 grams; 0.028 mole), and 2-nitroamino5,5-dimethyl-1,3-diazacyclohex-2-ene (5.0 grams; 0.029 mole). The resulting mixture is heated to 95° C. over a period of 20 minutes, and stirred thereat for 2 hours. Additional hydrazine hydrate (0.94 gram; 0.0187 mole) is then added to the reaction mixture, and heating at 95° C. is continued for an additional 24 hours. The slurry is then cooled to room temperature and the precipitate is isolated by filtration, washed with 1-propanol (20 mls) and dried under a vacuum at 50° C. to obtain 3.55 grams (68.5% of theoretical) of the desired product. Evaporation of the filtrate affords a second crop (1.5 grams) of the same compound. The total yield in two crops is 96.5% of theoretical. The infrared absorption spectra of the two crops are identical with that of 2-hydrazino-5,5-dimethyl-1,3-diazacyclohex-2ene monohydrochloride.
불러오는 중…
