Dr. Raminder Mulla, Lead Scientist, at Sygnature Discovery’s Nottingham laboratory, oversaw two workflows focussing on the oxidation of an aniline to a nitrate and the safe reaction of neopentyl iodide with t-butyllithium at scale. Asia was able to provide an easy-to-use chemistry platform that gave Sygnature Discovery greater control over their process than traditional batch reactors, both reducing the cost and risk associated with these applications.

Case study 1: Oxidation of an aniline to a nitroarene

Dr. Mulla and the team concluded that the hundreds of grams quantities of mCPBA they required coupled with the process temperatures of over 80°C presented a substantial explosion risk if the process was run in a conventional batch reactor.

Asia was selected as the best flow option to run this process due to its open standards for fluidic fittings, allowing for easy interfacing with non-Syrris equipment such as a custom 50 mL tube reactor developed by the team to reach the required residence times. The Asia Syringe Pump’s comprehensive emergency cut-out feature and highly accurate, consistent dosing of the pump heads, along with the ability to handle the high back-pressures associated with superheated solvents provided an invaluable tool in completing the process.

We couldn’t run oxidation of an aniline to a nitroarene at the desired scale in batch reactors as oxidant would accumulate and possibly detonate. Asia provided us with an easy-to-use flow chemistry platform in which to perform this scale-up, including a syringe pump capable of working against high back-pressures and modules such as the chip heater that could be adapted to work with third party equipment.

Download the case study to discover more about the process and how Asia allowed Sygnature Discovery to scale up their process by 83% yield after workup.

Case study 2: t-Butyllithium

Sygnature Discovery’s second case study using Asia, describes the safe reaction of neopentyl iodide with t-butyllithium. The use of t-butyllithium was deemed necessary as part of a synthesis requiring reaction of a neopentyl organometallic with an unreactive electrophile on a decagram scale. T-butyllithium is a reagent with significant safety and handling concerns due to its pyrophoricity, and there are currently limited examples of it being used in flow chemistry.

Dr. Mulla and the team found that running this process in batch led to chromatographically inseparable impurities impacting the product profile and lowering yield. Thus, running in batch increased the t-BuLi requirement and introduced high-risk operations. Asia was selected to perform the scale-up process as it allows for dosing of t-BuLi directly from the bottle, provides comprehensive safety features including the ability to stop dosing all reagent streams in cases of blockage, and offered universal compatibility with third party equipment, allowing key modifications to be made to the reactor setup. Asia Syringe Pump’s safety protocols along with the complete infusion of the contents of each syringe, making for efficient purging, also added to the simplicity of scaling up in flow.

Scaling up with Asia was a simple process where we ran the system for longer periods to get our desired results. Asia Syringe Pump’s complete infusion of the syringe contents made purging of residual t-BuLi reagent an easy process, allowing for a highly controlled, productive, synthesis.

Download the case study to discover how Asia allowed Sygnature Discovery to safely scale-up reaction of neopentyl iodide with t-butyllithium.

Asia is a versatile flow chemistry platform that can support easy scale up of a vast range of chemistry applications. As Sygnature Discovery found, Asia truly enables more chemistry to be done, allowing the user to mitigate risk through enhanced process control, reducing the need for large volumes of reagents, and enabling sophisticated , rapid optimization of processes that would be challenging in conventional batch reactors.

Syrris give us excellent customer support and are always friendly, responsive, and take an interest in our applications. They always work to make the Asia system work for us.

Further reading on flow chemistry

• Syrris flow chemistry applications guide
• Syrris continuous fow reactors guide
• Syrris laboratory syringe pump guide

Have a specific question about continuous flow chemistry, or want to know more about Asia or any other Syrris products? Fill in our contact form and a member of the Sales team will be in touch.