Synthesis Of Hexane Lab Report
Procedure
2.0 g of Mo(CO)6 and 10 mL of mesitylene were added into a 50-mL round bottom flask along with a small magnetic stir bar. A 30-cm reflux condenser was attached to the round bottom flask and a gas inlet was then connected to the condenser and to the bubbler. Since Mo(CO)6 and the product tends to react with oxygen at high temperatures this reaction must take place in an inert atmosphere. Therefore, the gas inlet was connected at the top of the condenser to a nitrogen source and was flushed with a stream of nitrogen of approximately 5 minutes. A rheostat-controlled heating mantle was used to heat the solution at a moderate boil for 30 minutes. During the boiling period, the solution turned to a darkish green color. After the 30 minutes were up the heating mantle was immediately removed and N2 was turned on until the solution cooled to room temperature. The solution was washed with 15 mL of hexane via vacuum filtration and then another 5 mL of hexane was added to wash the solution. About 20 mL of CH2Cl2 was used to purify the crude …show more content…
IR ATR spectra of the solid complex was acquired along with a solution cell IR of the complex in methylene chloride. According to the lab manual used for this experiment two characteristic carbonyl IR stretches of MesMo(CO)3 occur strongly around 2000 cm-1. The stretches at 1940 and 1855 cm-1 in the IR ATR spectra are possible indicators of carbonyl stretches in the compound that was made. The solution cell IR spectra had two stretches at 1981 and 1876 cm-1 are also indicative of carbonyl stretches in the compound that was made. The IR ATR spectra that was collected has a similar carbonyl stretch pattern similar in the (benzene)chromium tricarbonyl IR spectra found in the literature (figure 1)2. The stretches of the carbonyls of the chromium tricarbonyl complex at 1942 and 1833 cm-1 are near 2000
2.0 g of Mo(CO)6 and 10 mL of mesitylene were added into a 50-mL round bottom flask along with a small magnetic stir bar. A 30-cm reflux condenser was attached to the round bottom flask and a gas inlet was then connected to the condenser and to the bubbler. Since Mo(CO)6 and the product tends to react with oxygen at high temperatures this reaction must take place in an inert atmosphere. Therefore, the gas inlet was connected at the top of the condenser to a nitrogen source and was flushed with a stream of nitrogen of approximately 5 minutes. A rheostat-controlled heating mantle was used to heat the solution at a moderate boil for 30 minutes. During the boiling period, the solution turned to a darkish green color. After the 30 minutes were up the heating mantle was immediately removed and N2 was turned on until the solution cooled to room temperature. The solution was washed with 15 mL of hexane via vacuum filtration and then another 5 mL of hexane was added to wash the solution. About 20 mL of CH2Cl2 was used to purify the crude …show more content…
IR ATR spectra of the solid complex was acquired along with a solution cell IR of the complex in methylene chloride. According to the lab manual used for this experiment two characteristic carbonyl IR stretches of MesMo(CO)3 occur strongly around 2000 cm-1. The stretches at 1940 and 1855 cm-1 in the IR ATR spectra are possible indicators of carbonyl stretches in the compound that was made. The solution cell IR spectra had two stretches at 1981 and 1876 cm-1 are also indicative of carbonyl stretches in the compound that was made. The IR ATR spectra that was collected has a similar carbonyl stretch pattern similar in the (benzene)chromium tricarbonyl IR spectra found in the literature (figure 1)2. The stretches of the carbonyls of the chromium tricarbonyl complex at 1942 and 1833 cm-1 are near 2000