The invention provides a preparation method of 3, 6-
diacetylene carbazole, and relates to the technical field of
organic synthesis. According to the preparation method, 3, 6-diiodocarbazole and Boc2O are taken as initial reaction raw materials for reaction, then the initial reaction raw materials react with 2-methyl-3-butyne-2-
alcohol, and finally, 3, 6-diethynyl
carbazole is obtained through deprotection reaction. According to the preparation method, an NH group in 3, 6-diiodocarbazole is protected by Boc2O, then the protected 3, 6-diiodocarbazole reacts with 2-methyl-3-butyne-2-
alcohol, so that the reaction is very easy to occur, byproducts are few, the product yield is greatly improved, and the 3, 6-diethynyl
carbazole is prepared through a
protecting group removal reaction. The method has the advantages of high total yield of 3, 6-diethynyl carbazole, few
system byproducts, easiness in post-treatment, low production cost and suitability for industrial production. The test result of the embodiment shows that the total yield of the 3, 6-
diacetylene carbazole is 81.3% or above.