In the fine chemicals industry, development is driven by a constant strive for higher yields and selectivity of existing processes and faster development of new processes and products. Key constraints in process development in today's low-tonnage chemicals sectors (fine and effect chemicals) remain the time and cost spent obtaining data to identify and verify new processes. This often limits the amount of knowledge of the process chemistry acquired from any process development activity. In the present work, the capability of a simple high throughput experimental device is exploited to develop, apply and evaluate some laboratory-based tools to provide valuable insights into the process chemistry, especially in the critical early stages of process development. This paper discusses the experimental and modelling approaches (based on a model heterogeneous solid-catalysed acylation reaction) adopted to investigate a set of conditions that should deliver good process performance. The use of the experimental design and data reconciliation concepts in an integrated way to deliver a better process design is also demonstrated.