The purpose of this work is to investigate the influence of n-hexane addition on in situ transesterification of a solid raw material for biodiesel production. Extraction and reaction of macroalgae oil has been performed simultaneously in a batch reactor adding n-hexane with the reactants. In order to analyze the influence of n-hexane on the transesterification, the reaction was also carried out with sunflower oil. The results show that the presence of n-hexane does not have an important effect on the transesterification. It was also observed that this method requires large quantities of methanol to carry out the reaction. The best reaction conditions for in situ transesterification of marine macroalgae were 300:1 methanol-to-oil molar ratio, 1% catalyst concentration, 60 °C reaction temperature and 11 h reaction time, resulting in a methyl esters yield of 17.1%. Thus, biodiesel production from macroalgae by transesterification in situ could be feasible, using hexane for the extraction and eliminating the previous extraction. This integrated method is thus effective and technically attractive.