Reaction Including Metal Reagent

 Reaction including metal reagent usually generate heat and gas! Be careful! Last Friday I had run one reaction which is about the 1,4-Addition of 1,3-Diesters to Conjugated Enones by In/TMSCl. When indium was added to THF, nothing tooks place but just leading to one suspension. When diethyl bromomalonate was added, still nothing happened. However, when TMSCl was added to the above mixture, huge amount of heat and gases were produced. So the reaction mixture just overflowed from the RBF. Fortunately it was just a small scale reaction. If it were a large scale reaction,the consequence will be awful.

 

So one standard reaction apparatus should including condenser, Argon outlet, addition funnel and stirrer. 

 

Another thing be worth noting is when the reaction was complete it was quenched by saturated NaHCO3. Because there is large access of TMSCl in the reaction, so huge amount of CO2 was produced. So once again, quenching should be conducted very slowly.