Single Reaction Chamber (SRC) Technology
How It Works
SRC operation is extremely simple and completely automated from start to finish. A simple reaction rack, similar to a rotary auto sampler rack, is loaded with one or several reactions weighed into glass vials. The vials are capped with loose fitting Teflon caps (to prevent condensation from the top of the SRC chamber dripping into the vials). The rack is fitted to the chamber top and mechanical stirrer, which is lowered automatically into the chamber.
The reaction vials sit in a microwave absorbing liquid pool that provides a consistent “load” for the delivered microwave energy and temperature monitoring. This insures even heating and consistent conditions from run to run. The chamber clamp is secured automatically and the chamber pressurized with N2 (typical: 40 bar). This prevents boiling of solvents as the run starts and essentially acts as a “cover” over the reaction, eliminating any possibility of cross-over of reacting substrates or solvents.
Intuitive User Interface The synthWAVE is operated via a control terminal featuring a full-color 6.5” touch screen display. The terminal runs Milestone’s renowned EasyCONTROL software, which enables simple and intuitive, but extremely flexible and powerful control over the reaction process. Method setup could not be simpler: set target temperature, ramp time and hold time. Press ‘Start,’ and the system automatically follows the desired temperature profile, continuously varying the microwave output via a sophisticated Proportional Integral Derivative (PID) controller, regardless of reagent volume or number of vials in the run. EasyCONTROL features full audit trail capability plus multi-level user access security: each operator has a personal password to access the software.
Run data are stored on a flash drive or USB memory stick and can be transferred to a PC with the optional EasyDOC software. The software also controls a powerful stirrer, which ensures vigorous stirring in the 1L PTFE vessel, or in all vials whenever a rack is used, thus assuring reliable and consistent results.
At the heart of the synthWAVE is a Teflon-lined 1 liter stainless steel reaction chamber, which serves both as a microwave cavity and a reaction vessel.
Samples are weighed into vials, and suitable reagents are added. Vials are placed in a rack, which is automatically lowered into the reaction chamber. The chamber is sealed and pre-pressurized with inert gas, which physically acts as a cap for the vials, avoiding boiling of the solutions and preventing cross contamination. At the completion of the microwave run, a built-in cooling device rapidly lowers the temperature.
1. Analog Pressure Gauge
2. Gas Inlet
3. Gas Outlet
4. Clamps
5. Overhead Stirrer
6. Gas Release Valve
7. Dewar Flask
8. In-situ Sampling
9. Exhaust System
10. Temperature Sensor
Easy Scale Up
The combination of high microwave power density of 1.5kW/L and powerful stirring allows the same conditions developed for small-scale reactions to be replicated.
Faster Screening
Multiple reactions are carried out simultaneously under exactly the same temperature and pressure conditions - even using different solvents. This enables a quick and easy evaluation of different catalysts, solvents and reaction conditions.
Easy Sampling
Easily and conveniently sample reaction products at any time during the experiment.
Operate Under Modified Conditions
Simply add an inert gas to achieve an inert environment. Add hydrogen or oxygen to produce a reducing or oxidizing atmosphere respectively. Speed up reactions with gas molecule insertion using gases such as CO or CO2.
Example: the preparation of isocyanates derivatives by the Staudinger-Aza-Wittig reaction.
High Pressure Capability
The synthWAVE allows for the use of a wider range of low-boiling reagents, reactants and solvents. Perform aqueous reactions and extractions below boiling point. Extremely efficient cooling of the reaction vessel avoids or minimizes degradation and side reactions.
