1-Bromobutane
Experimental procedure for the synthesis
The experimental procedure of the synthesis of 1-bromobutane performed was based on protocols H and I, where it is suggested a procedure at microscale and other similar at macroscale. The only difference is that the use of p-xylene as auxiliary substance is only prescribed in the procedure at microscale (protocol H). This substance has the function of collecting any product that becomes attached to anhydrous calcium chloride when drying. Although the use of p-xylene is not suggested in the macroscale procedure, this was performed in the present study to have a better control of the variables under study.
The synthesis performed presents a complex experimental procedure, with several steps. After the mixture of the stoichiometric reagents, a reflux followed by a simple distillation are carried out, where some unwanted products can be separated such as, for example, sodium hydrogen sulphate and sulphuric acid. The liquid collected in the distillation is then washed with water, sulphuric acid and sodium hydroxide by liquid-liquid extraction to be isolated from other substances (but-1-ene, dibutyl ether and butan-1-ol that does not reacted). Finally, the product is dried with anhydrous calcium chloride and purified by simple distillation.
Documents to support students (detailed protocols of the procedures and a document to assess greenness) are available in the links below.
Experimental procedure at macroscale
