We report herein the fabrication of a simple and price-affordable portable reaction station for use in parallel solution-phase synthesis. This homemade device uses currently available laboratory components and equipment. Specifically designed to fit standard magnetic hotplates/stirrers, it can simultaneously hold up to 24 heated and magnetically stirred glass reactors of both 10 and 50 mL capacities. Glass reactors are connected by flexible 16-gauge metal needles to a central gas manifold equipped with an inlet/outlet for vacuum and inert gases. Reaction temperatures can be optimally varied from -78°C to 150°C. Using a statistical screening DOE method, this parallel array reactor station has been successfully operated to optimize the one-step deprotective O-formylation of a sterically hindered bis-O-tert- butyldiphenylsilyl (O-TBDPS) aromatic diol. The latter transformation was mediated by the Vilsmeier-Haack reagent POCl3·DMF using a range of Lewis acid and metal salt promoters, including their binary combinations.
|Number of pages||10|
|State||Published - May 2006|
- High-throughput experimentation
- O-Formate esters
- O-silyl ether deprotection
- Statistical design of experiments (DOE)
- Vilsmeier-Haack reagents