This preview shows page 1. Sign up to view the full content.
Unformatted text preview: C -4.5oC 54.09 g/mol Cyclohex-4-ene1,2-dicarboxylic
C8H8O3 97103oC NaOH 318oC 152.15 g/mol 1,388oC Petroleum Ether Xylene
C6H4(CH3)2 39.99 g/mol 30-50oC 137-140oC Toluene
C6H5CH3 Experiment: -93oC Structure 110-111oC 92.14 g/mol Na-OH To begin the experiment, a sand bath was set up on a hot plate and a thermometer was
added and held upright by a clamp. The hot plate was set on high, and once the temperature
reached 190oC it was maintained between 150-200oC. Approximately 0.207 grams of butadiene
sulfone was measured and placed into a 4.0mL conical vial. Next, 0.095 grams of maleic
anhydride was measured and placed inside the same 4.0mL conical vial. A 1 mL pipet was then
used to add 0.25 mL xylene to the conical vial along with two boiling stones. The drying tube
was then prepared with Sodium hydroxide pellets and cotton. All of the joints of the drying tube
were greased and the reflux apparatus was assembled as seen in Figure 3.
The sand bath was still hot and at 150oC when the conical vial was placed in it with the
condenser secured. The solution in the conical vial was clear and began to boil at 190oC, when
the reflux began, and boiling was maintained for 25 minutes. After 25 minutes reflux ended and
the temperature was still 190oC. The heating of the sand bath continued at 150oC. The vial was
removed from the sand bath and allowed to cool to room temperature. The solution now had a
slight yellow tint. Once cooled, approximately 0.5 mL of toluene was added to the conical vial
and the solution turned clear and everything in the solution dissolved. Then approximately 0.5
mL of petroleum ether was then added to the conical vial and the solution turned cloudy. The
solution was stirred to form one, homologous cloudy layer and the vial was placed back on the
sand bath and heated at 150oC for approximately 15 minutes until the solution was only slightly
cloudy, allowing all particles to dissolve.
After 15 minutes the conical vial was removed from the sand bath and allowed to cool to
room temperature. Once cooled, the vial was placed on ice to induce...
View Full Document