Our focus was to enable the autonomous execution of crucial synthetic steps, particularly emphasizing workup, and isolation methods such as distillation, crystallization, and liquid ̶ liquid extraction. Aside from column chromatography, which is undesirable in process chemistry, the abovementioned methods encompass the primary unit operations involved in compound isolation after a synthetic operation. However, their automation is hindered by the aforementioned challenges discussed in the introduction. To showcase the performance and adaptability of HeinSight2.0, we have chosen a series of progressively challenging case studies for each of these key isolation strategies.