Basic procedure for inert atmosphere reactions

A typical simple reaction set-up using a manifold is shown in Fig. 9.1 and the following general procedure is applicable to a wide range of reactions. However, this is only intended to be a general guide and can easily be modified to suit various requirements. Some of these modifications are discussed later in this chapter. 

Before starting, decide on the order for addition of reagents and if possible arrange this so that any solid reagent is added first. If this is not possible try to add the solid as a solution, using the technique described later. If a reagent really does have to be added as a solid, this can be done successfully and again a method will be described to do this. 

Make sure before you start that you have aU the dry syringes, needles, and any other ancillary items, and that you are familiar with the operation of the manifold and the 3-way Quickfit tap (Fig. 9.2). 

At this stage the reaction flask can be immersed in a cooling bath and stirred with a magnetic stirrer. Never cool a flask before it is under the inert atmosphere as this causes moisture to condense. 

The reaction can easily be monitored by tic, gc, etc. Again increase the inert gas flow through the manifold so that rapid bubbling is maintained as the 3-way tap is opened to position B, then insert a 

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