Abstract
We have developed a single-mode microwave reactor for continuous-flow synthesis with various methods of operation. This device measures the resonant frequency and modulates the oscillation frequency accordingly to maintain the maximum electric field intensity in the cavity. It can be operated either using constant applied irradiation power or using new programs which change the electric power (E-GRA) and change the flow rate (Fl-GRA), in order to rapidly screen various reaction conditions. As a model reaction, the Claisen rearrangement reaction of allyl 1-naphthyl ether 1 was rapidly optimized in this device, affording the desired product 2-allylnapthalen-1-ol 2 in high (91%) yield and up to 20 g/h productivity.
Highlights
Organic reaction systems are heated by external heaters such as oil baths
The number of reports on organic synthesis using MW heating has grown in the past decades [5, 6]
We previously reported a single-mode MW device for continuous-flow synthesis (MW flow reactor), with a resonator in which the electric field is well-amplified and wellcharacterized [45]
Summary
Organic reaction systems are heated by external heaters such as oil baths. The boiling of CPME was prohibited by the back pressure regulator set to 2.5 MPa. to control the temperature of the flow channel, heating was carried out under a constant flow rate and stepped applied power (E-GRA method).
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