Methods of synthesis of 1,3-diacyloxy benzene and 1,4-diacyloxy benzene derivatives are discussed. The compounds of first series was synthesized by different acid chlorides (Lauric, myristic,palmitic, heptadecanoic and steric) on treatment with resorcinol in presense of triethyl amine we can get 1,3-diacyloxy benzene derivatives and it was characterized by I.R and NMR data. The compounds of second series was synthesized by different acid chlorides on treatment with hydroquinone in presense of triethyl amine, resulting the formation of 1,4-diacyloxy benzene derivatives and characterized by I.R and NMR. The above two series of compounds was purified and crystallized from alcohol as shining needles. Further the liquid crystalline properties were studied for the above two series of compounds by using DSC and all the compounds posses pronounced L.C. Properties and showed the mesophase at two transition temperature regions. The mesophases were photographed and respective thermograms were recorded during heating rate 50/min and 100/min on cooling. The results are presented.