Attach the distilling column and glass absorption trap as shown in Figure 7.3. Add 2-3 boiling chips and
heat the flask to a gentle reflux using a setting of about 60 on the rheostat. Again, the exact setting depends on
the size of the heating mantle, etc. Do not heat too quickly as the reaction can get out of control and HBr gas
can escape. If you do see HBr gas escaping immediately lower the heating mantle from the flask and call for
assistance from your instructor or teaching assistant.
Once all of the solid sodium bromide has dissolved, continue heating the reaction at a gentle reflux for
about 30 minutes longer. You will see two layers separate. The yellowish brown layer on top is 1-
bromobutane. It is not soluble in the aqueous H2SO4 layer on the bottom.