Synthesis of graphene via the deoxygenation of the graphite oxide (GO) is a method for the large-scale production of this nanomaterial possessing exceptional mechanical, electrical and translucent properties. Graphite oxide sheet contains at least four different oxygen atoms connected to the Csp3 and Csp2 atoms of the sheet in the form of hydroxyl, epoxy, carboxyl or carbonyl groups. Some of these functional groups are located at the surface but others situated at the edges of the platelets. To obtain the graphene nanoplatelets or the few-layer graphene the oxygen functionalities must be removed. Exfoliation and deoxygenation can be accomplished by the use of chemical reductants or heat. Thermal deoxygenation as greener and simpler approach is more preferable over chemical reduction approach. Usually a considerable mass loss of GO observed upon heating at temperatures starting at 200 °C and is attributed to the deoxygenation process. In order to avoid the defects of the obtained graphene sheets it is very important to find the methods for lowering the deoxygenation temperature of GO. Herein, we have investigated the way treatment of the Hummer's synthesis product with acetone and methyl tert-butyl ether under ultrasonication in order to lower the thermal stability of the graphite oxide and its deoxygenation temperature. The obtained results indicate that treatment of the graphite oxide with solvents mentioned above substantially reduces the reduction and exfoliation temperature (130 °C) under ambient atmosphere. The investigation of the composition of evolved gases by hyphenated Pyr/GC/MS method at different experimental conditions under helium atmosphere shows that without the expected H2O, CO and CO2 also sulphur dioxide and acetone has been released.