A process of making biodiesel from crude tall oil by reacting crude tall oil with a C.sub.1-C.sub.6 alkanol in the presence of an acid catalyst or by reacting crude tall oil with an acyl halide in the presence of a C.sub.1-C.sub.6 alkanol. The reaction product of either of these reactions is separated into a suspension liquid by the addition of a polar liquid. The biodiesel product is recovered from the suspension liquid by addition of an organic solvent which produces a polar liquid phase and an organic liquid phase. The biodiesel is recovered from the organic liquid phase by evaporating the organic solvent, which is recovered for use in subsequent separation processes, and vacuum distilling off the product biodiesel from the organic solvent-free organic liquid phase.