Procedure Of A Sand Bath

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Procedure: A sand bath was set atop a hot plate set at power level 5, while a 10 mL round bottom was prepared with the addition of 14 (0.33 mL) drops of olive oil and 1 mL of cyclohexene. Once the contents of the 10 mL round bottom were mixed thoroughly, a boiling chip was added, and the round bottom was attached to a reflux condenser apparatus. The reflux was run for 20 minutes starting at the point in time when the mixture within the round bottom flask (that was submerged in the heated sand bath) began to boil. While the running the reflux, a 5 ¾ inch Pasteur pipette was obtained and clamped vertically with the tip facing downward. A small amount of glass wool was placed inside of the pipette and pushed down to block the narrowing end by a wooden boiling stick. A total of 100 mg (0.100 g) of celite was weighed out and was carefully added into the pipette as an additional layer atop the glass wool stopper. Once the 20 minutes elapsed, the reflux-round bottom apparatus was removed form heated sand bath and let to cool to room temperature. At the point in which the round bottom and its content reached room temperature, 2 mL of dichloromethane was added. A clean test tube was placed under the prepared celite-containing Pasteur pipette to collect all of the filtered content of the mixture pipetted into the top of the column from the round bottom flask. After the full contents of the round bottom was pipetted into the filtration column, the collected content in the test tube was poured into a different (clean) round bottom flask for rotary evaporation. Post rotary evaporation, the round bottom was placed into an ice bath. Approximately 1-2 minutes after the round bottom was placed in an ice bath to cool, 2.0 mL of dichloromethane we... ... middle of paper ... ...lor in the bromine test when attempting to detect the presence of the product were successful as well as the overall process of product purification via celite column. However, the yield shows inaccuracies inherently as it is a nonsensical concept to have over 100.0% yield which is already challenging to achieve. The identified issues with the post-rotary evaporation product not solidifying further may be one contributing factor, however, the main contributing factor in the resulting nonsensical calculations of percent yield may be explained by the fact that the theoretical yield was not calculated on an absolute basis in the first place. Thus, the issues concerning the calculated value of final percent yield may be purely attributed to the vague nature of the theoretical yield approximation that would directly impact the final calculation of overall percent yield.
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