Method for synthesizing diaza-bridged compound and a diaza-bridged compound
The present disclosure discloses a method for synthesizing a diaza-bridged compound and a diaza-bridged compound, belonging to the field of organic synthesis. The present disclosure includes the following reaction: in the formula, R is aryl, substituted aryl, alkyl or haloalkyl, R a is any one of H, 2-nitrobenzenesulfonyl, 4-nitrobenzenesulfonyl or 2,4-dinitrobenzenesulfonyl, n=1 or 2. Since compound 2 and NH 3 are used as raw materials, the present disclosure can not only effectively shorten the process flow and save process costs, but also improve the reaction yield to a certain extent. The present disclosure also provides a diaza-bridged compound, where the structural formula thereof is in the formula, R a is any one of 2-nitrobenzenesulfonyl, 4-nitrobenzenesulfonyl or 2,4-dinitrobenzenesulfonyl. Since the compound has a higher melting point, is easy to recrystallize to get solid and not easy to form oil under high temperature, the diaza-bridged compound is suitable for long-distance transportation and long-term storage.
1. A diaza-bridged compound having a structural formula of:
wherein in the formula, R a is any one of 2-nitrobenzenesulfonyl, 4-nitrobenzenesulfonyl, or 2,4-dinitrobenzenesulfonyl.
2. The diaza-bridged compound according to claim 1 , wherein R a is 2-nitrobenzenesulfonyl.
3. The diaza-bridged compound according to claim 1 , wherein the compound is obtained by recrystallization.
4. The diaza-bridged compound according to claim 3 , wherein recrystallization of the compound comprises the following steps:
dissolving the diaza-bridged compound in solvent A, then
adding solvent B,
mixing evenly,
precipitating a crystal at −50° C. to −10° C., and then
filtering the crystal to obtain a recrystallized diaza-bridged compound,
wherein:
the solvent A is any one of carbon tetrachloride, chloroform, ethyl acetate, acetone, ethanol, methanol, dichloromethane, 1,2-dichloroethane, trichloroethylene, tetrahydrofuran, 2-methyltetrahydrofuran, ethyl formate, methyl acetate, isopropyl acetate, acetonitrile, propionitrile, or carbon disulfide, and
the solvent B is any one of petroleum ether, n-hexane, cyclohexane, benzene, diethyl ether, isopropyl ether, n-pentane, n-heptane, propyl ether, nitromethane, or nitrobenzene.