Chemistry Experiment Instructions
Procedure.
1) Accurately weigh approximately 2 g of the mix and dissolve it in 50 mL of diethyl ether. Be sure to dissolve the entire mix since it is not homogeneous.
2) Pour the solution into a separatory funnel.
3) To extract the nicotinamide from the mixture, add 5 mL of 5% HCl and shake gently. Draw off the lower aqueous layer into 125 mL Erlenmeyer flask and repeat the extraction with a second portion of HCl. Combine the three extracts and then set this mixture aside.
4) To separate the trans-cinnamic acid from the mixture, extract the ether solution twice with 5 mL of 5% sodium bicarbonate. Combine the extracts and set aside.
5) After neutralizing the aqueous solutions, filter or back extract with dichloromethane to obtain the separate compounds.
6) Pour out the remaining ether solution (which should contain only the 4-phenylphenol) through the neck of the separator funnel into a small Erlenmeyer flask. If any water droplets are visible, remove them before adding the drying agent. Add a small amount of anhydrous sodium sulfate (or magnesium sulfate) to the flask. Let the mixture stand for 5 min. occasionally swirling it gently.
7) Decant or pipette the organic liquid away from the drying agent and place it in a clean, dry Erlenmeyer flask. Place it in the hood to allow the ether to evaporate (if needed, set aside overnight to dry).
8) After separating the mix, collect the products by vacuum filtration. Wash with small amounts of distilled water.
9) Determine the mass and the identity of the major products by melting point.
10) Run a TLC for the qualitative analysis of the reaction products.
1) Accurately weigh approximately 2 g of the mix and dissolve it in 50 mL of diethyl ether. Be sure to dissolve the entire mix since it is not homogeneous.
2) Pour the solution into a separatory funnel.
3) To extract the nicotinamide from the mixture, add 5 mL of 5% HCl and shake gently. Draw off the lower aqueous layer into 125 mL Erlenmeyer flask and repeat the extraction with a second portion of HCl. Combine the three extracts and then set this mixture aside.
4) To separate the trans-cinnamic acid from the mixture, extract the ether solution twice with 5 mL of 5% sodium bicarbonate. Combine the extracts and set aside.
5) After neutralizing the aqueous solutions, filter or back extract with dichloromethane to obtain the separate compounds.
6) Pour out the remaining ether solution (which should contain only the 4-phenylphenol) through the neck of the separator funnel into a small Erlenmeyer flask. If any water droplets are visible, remove them before adding the drying agent. Add a small amount of anhydrous sodium sulfate (or magnesium sulfate) to the flask. Let the mixture stand for 5 min. occasionally swirling it gently.
7) Decant or pipette the organic liquid away from the drying agent and place it in a clean, dry Erlenmeyer flask. Place it in the hood to allow the ether to evaporate (if needed, set aside overnight to dry).
8) After separating the mix, collect the products by vacuum filtration. Wash with small amounts of distilled water.
9) Determine the mass and the identity of the major products by melting point.
10) Run a TLC for the qualitative analysis of the reaction products.