Highly Controlled Gas/Liquid Processes in a Continuous Lab‐Scale Device

Abstract

The use of reactive gases for syntheses on small laboratory scale is often avoided due to safety concerns so that expensive alternatives are required. The recent development of gas-permeable membrane-based reactors offers new options for safe handling of these gases in a continuous-flow system. A prototype of a gas/ liquid system was built to introduce gas in the microreactor. An integrated gas flow controller and inline FTIR analysis were used to safely handle the gas. With the system, the carboxylation of a Grignard reagent with carbon dioxide was chosen as a nonhazardous model reaction to validate the prototype reactor.

Using Carbon Dioxide as a Building Block in Continuous Flow Synthesis

“…[40] Theses tudies evaluated pre-saturatedC O 2 in THF (System 1) and continuous saturation systems (System2). [40] Theses tudies evaluated pre-saturatedC O 2 in THF (System 1) and continuous saturation systems (System2).…”

Managing Hazardous Reactions and Compounds in Process Chemistry

“…Reaction of the Grignard reagent with carbon dioxide to give a carboxylic acid in flow with a gas-permeable membrane reactor provides a simple process that can be monitored by IR (199).…”

4. Technology overview/Overview of the devices

“…Examples of liquid-phase reactions include Prilezhaev dihydroxylations [36], Vilsmeier-Haack formylations [37], while the principle of using gases at a very small scale in continuous mode was introduced, and an example was given with a Grignard Brought to you by | New York University Bobst Library Technical Services Authenticated Download Date | 7/15/15 2:14 AM model reaction [38]. The latter example includes direct coupling to FTIR equipment, extensively investigated earlier by Stephen Ley's group [39].…”