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The setup of the glassware for reflux used is shown in Fig 20.1. Note: the presence of the guard tube on the top of the reflux condenser. The distillation setup is shown in Fig 20.3.
The single shot equipment is shown in Fig 20.2. The distillation set-up shown in Fig 20.3
As with all chemical processes, care and attention to detail was needed at all times. The equipment was clean and dry before use. Many of the liquids used in the synthesis were flammable and naked flames were not used. Heating of the reaction vessel was by way of an electric hotplate. The most dangerous substances used in the process were metallic sodium and the strongly basic intermediary sodium ethoxide. Standard organic chemistry texts (eg. Solomons & Fryhle, 2004) spell out the dangers of handling these substances.
CAUTION: Sodium must be handled with great care and under no circumstances should the metal be allowed to come into contact with water as an explosion and fire may result. Sodium is stored under paraffin or xylene and should only be handled with tongs or tweezers, not with fingers.
Small waste or scrap pieces of sodium can be disposed of by placing them in a bottle containing large quantities of methylated spirits.
The commercial sodium is covered with a non-metallic crust. A sodium press can be constructed to remove this and produce clean sodium wire for the reaction vessel. See ‘Betty cooks with Sodium’).