Preparation
1,3-Adamantanediamine synthesis: 1,3-Adamantane dicarboxylic acid (12 g) was mixed with 50 mL of SOCl2 and the mixture was refluxed for 3 h. Excessive SOCl2 was evaporated and 1,3-adamantane dicarbonyl dichloride was obtained as white solid, dissolved in dried benzene and added to cold ammonia solution slowly, during which a white precipitate was formed gradually filtered and then washed the precipitate several times with water to give 1,3-disaminoacyladamantane as white solid, recrystallized from ethanol. White solid, yield 10.58 g (89 %).
Purification Methods
Purify it by zone refining. The dibenzoyl derivative has m 248o, and the dihydrochloride salt has m 310o (360o) after recrystallisation from aqueous EtOH or EtOH/Et2O. [Prelog & Seiwerth Chem Ber 74 1769 1941, Stetter & Wulff Chem Ber 93 1366 1960.]
