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【答案】应助回帖
wo357026239(金币+20, 翻译EPI+1): 2011-06-10 21:07:41
Five pyrene derivatives, including two bromine-containing compounds (1 - bromo pyrene and 1, 3, 6, 8- tetrabromo pyrene), 1 - pyrene acid, 1,3,6,8 - Tetra (trimethylsilyl acetylene) pyrene and one hydrogenated compound (1, 2, 3, 6, 7, 8 - hexahydro pyrene) were synthesized with pyrene as precursor. Synthesis methods of the above derivatives were listed as below.
1) 1 - bromo pyrene was obtained through single bromination of pyrene with limited bromine;
2) 1, 3, 6, 8- tetrabromo pyrene were obtained through tetra-bromination of pyrene with bromine of slightly higher than the theoretical amount of usage;
3) 1 - pyrene acid was obtained through reaction of 1 - bromo pyrene with N-BuLi and trimethyl borate at low temperature;
4) 1,3,6,8 - Tetra (trimethylsilyl acetylene) pyrene was obtained through reaction of 1, 3, 6, 8- tetrabromo pyrene with trimethylsilyl acetylene in the mix solvents of diisopropylamine and THF;
5) 1, 2, 3, 6, 7, 8 - hexahydro pyrene was obtained through hydrogenation of pyrene with hydrogen, which was supplied through reaction of sodium with isoamyl alcohol. Some of reactions were optimized and total five pyrene derivatives were analyzed with IR. |
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