Procedure: Synthesis of 1Bromobutane. Take a 25-mL round-bottomed flask. Dissolve 2.66 g of sodium bromide (solid, corrosive) in 3.

0 mL of DI water and 1.60 g of 1-butanol. Add a couple of boiling chips to the round bottom flask. Cautiously, with steady swirling, add 2.2 mL (3.8 g) of concentrated sulfuric acid drop wise to the solution (conc. H2SO4 is extremely corrosive and will cause severe burns if you get any on you skin). You should notice that the NaBr will dissolve once you start to heat the reaction mixture. Reflux the reaction using a sand bath for 45 min. Make sure reactants dont evaporate out of the condenser during the reflux (make sure that water is flowing through the condenser, throughout the reflux).
Clamp Water Out Condenser Water in Round bottom flask with boiling chips

Transformer

Gray Heating Mantle with sand

Stick a wad of glass wool on the top of the condenser to prevent vapor from escaping. As time proceeds you should see the formation of your product as a separate layer on top of the aqueous layer. After the 45 minutes of reflux, distill (simple distillation) the product (from ~60-95 0C) into a large test-tube until no more waterinsoluble droplets are seen to collect in the test-tube. One lab partner should wash the round-bottomed flask and the distillation apparatus as soon as the distillation is done and the apparatus has cooled down. The other lab partner should move the distillate to a small disposable test-tube. Rinse the larger test-tube with about 1mL of water and transfer it to the same small disposable test-tube containing your product. Note that the 1-bromobutane now forms the lower layer. Remove the 1-bromobutane from above, with a plastic pipette, and place it in another dry small test-tube. Add 1mL of concentrated sulfuric acid, and mix the contents well by flicking the tube. The acid will remove unreacted starting material and any by-products. Allow the two layers to separate completely, and then remove the sulfuric acid layer (density: 1.841 g/mL; bottom layer) using a new plastic pipette. Wash the 1-bromobutane layer (density 1.275 g/mL) with 1mL of 3 M NaOH (density 1.11 g/mL). NaOH neutralizes any traces of H2SO4 in the organic product layer. At this point, your product layer will turn milky. Let the two layers separate out and remove the top NaOH layer with a new plastic pipette. Please save all layers until you are absolutely sure that you have the product in hand. Dry 1-bromobutane (product) by adding a small amount of anhydrous magnesium sulfate and mixing (glass rod) until the liquid clears. After 5 min, pour out the dried liquid into clean, dry and pre-weighed flask. Weigh the final product. Show your limiting reagent and calculate the theoretical yield and determine your percent yield (You need to show all work to get any credit!).