Experimental: A. Preparation of tetrakis(triphenylphosphine)copper(1) tetrafluoroborate, [Cu(PPH3)a]BF4 Reflux 0.114 grams (0.480 mmol) of Cu(BF4)2-nH2O and 0.755 grams (2.88 mmol) of triphenylphosphine in absolute ethanol (200 proof) (15 mL) until the color changes from blue to white. This change can happen fast; be sure to allow the solution to reflux 10 min after observing the color change. 1. After the reaction mixture is allowed to cool, isolate the complex by vacuum filtration using a glass fritted filter. Note that an ice bath may be necessary for full precipitation. 2. Determine the mass of the product. The precipitate contains [Cu(PPh3)4]BF4 as well as some co- precipitated PPH3. 3. В. Preparation of 2,9-Dimethyl-1,10-phenanthroline-bis(triphenylphosphine)copper(1) tetrafluoroborate 1. Add 0.500 grams (0.417 mmol) of the [Cu(PPH3)4]BF4 synthesized in Part A to a 250-mL round bottom flask with approximately 100 mL of anhydrous diethylether. In a separate beaker, dissolve 0.0723 grams (0.347 mmol) of 2,9-dimethyl-1,10-phenanthroline (DMP) in approximately 20 mL of diethylether. If the DMP does not dissolve fully in the ether, add a minimal amount of ethanol to aid in the dissolution. 2. 3. Slowly add the DMP solution to the copper solution over a period of 30 minutes. Allow the solution to stir for approximately one hour following the addition of DMP. 4. The progress of the reaction can be followed by the use of a UV-handlamp. The triphenylphosphine will glow purple. As the mixed ligand complex forms the solution will glow an orange or yellow color. 5. Isolate the solid product via vacuum filtration. 6. Wash the product repeatedly with ether to remove any excess triphenylphosphine still present. 7. Weigh the [Cu(DMP)(PPH3)2]BF4 obtained and calculate the percent yield.
Experimental: A. Preparation of tetrakis(triphenylphosphine)copper(1) tetrafluoroborate, [Cu(PPH3)a]BF4 Reflux 0.114 grams (0.480 mmol) of Cu(BF4)2-nH2O and 0.755 grams (2.88 mmol) of triphenylphosphine in absolute ethanol (200 proof) (15 mL) until the color changes from blue to white. This change can happen fast; be sure to allow the solution to reflux 10 min after observing the color change. 1. After the reaction mixture is allowed to cool, isolate the complex by vacuum filtration using a glass fritted filter. Note that an ice bath may be necessary for full precipitation. 2. Determine the mass of the product. The precipitate contains [Cu(PPh3)4]BF4 as well as some co- precipitated PPH3. 3. В. Preparation of 2,9-Dimethyl-1,10-phenanthroline-bis(triphenylphosphine)copper(1) tetrafluoroborate 1. Add 0.500 grams (0.417 mmol) of the [Cu(PPH3)4]BF4 synthesized in Part A to a 250-mL round bottom flask with approximately 100 mL of anhydrous diethylether. In a separate beaker, dissolve 0.0723 grams (0.347 mmol) of 2,9-dimethyl-1,10-phenanthroline (DMP) in approximately 20 mL of diethylether. If the DMP does not dissolve fully in the ether, add a minimal amount of ethanol to aid in the dissolution. 2. 3. Slowly add the DMP solution to the copper solution over a period of 30 minutes. Allow the solution to stir for approximately one hour following the addition of DMP. 4. The progress of the reaction can be followed by the use of a UV-handlamp. The triphenylphosphine will glow purple. As the mixed ligand complex forms the solution will glow an orange or yellow color. 5. Isolate the solid product via vacuum filtration. 6. Wash the product repeatedly with ether to remove any excess triphenylphosphine still present. 7. Weigh the [Cu(DMP)(PPH3)2]BF4 obtained and calculate the percent yield.
Chemistry
10th Edition
ISBN:9781305957404
Author:Steven S. Zumdahl, Susan A. Zumdahl, Donald J. DeCoste
Publisher:Steven S. Zumdahl, Susan A. Zumdahl, Donald J. DeCoste
Chapter1: Chemical Foundations
Section: Chapter Questions
Problem 1RQ: Define and explain the differences between the following terms. a. law and theory b. theory and...
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I need help figuring out the balanced chemical equation of this reaction so that I can figure out the theoretical yield of the product.
![Experimental:
A. Preparation of tetrakis(triphenylphosphine)copper(1) tetrafluoroborate, [Cu(PPh3)4]BF4
Reflux 0.114 grams (0.480 mmol) of Cu(BF4)2·NH2O and 0.755 grams (2.88 mmol) of triphenylphosphine in
absolute ethanol (200 proof) (15 mL) until the color changes from blue to white. This change can happen
fast; be sure to allow the solution to reflux ~10 min after observing the color change.
1.
After the reaction mixture is allowed to cool, isolate the complex by vacuum filtration using a glass fritted
filter. Note that an ice bath may be necessary for full precipitation.
2.
3. Determine the mass of the product. The precipitate contains [Cu(PPH3)4]BF4 as well as some co-
precipitated PPH3.
B. Preparation of 2,9-Dimethyl-1,10-phenanthroline-bis(triphenylphosphine)copper(1) tetrafluoroborate
Add 0.500 grams (0.417 mmol) of the [Cu(PPH3)4]BF4 synthesized in Part A to a 250-mL round bottom flask
with approximately 100 ml of anhydrous diethylether.
1.
In a separate beaker, dissolve 0.0723 grams (0.347 mmol) of 2,9-dimethyl-1,10-phenanthroline (DMP) in
approximately 20 mL of diethylether. If the DMP does not dissolve fully in the ether, add a minimal
2.
amount of ethanol to aid in the dissolution.
3. Slowly add the DMP solution to the copper solution over a period of 30 minutes. Allow the solution to stir
for approximately one hour following the addition of DMP.
4. The
progress of the reaction can be followed by the use of a UV-handlamp. The triphenylphosphine will
glow purple. As the mixed ligand complex forms the solution will glow an orange or yellow color.
5. Isolate the solid product via vacuum filtration.
6.
Wash the product repeatedly with ether to remove any excess triphenylphosphine still present.
7. Weigh the [Cu(DMP)(PPH3)2]BF4 obtained and calculate the percent yield.
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Transcribed Image Text:Experimental:
A. Preparation of tetrakis(triphenylphosphine)copper(1) tetrafluoroborate, [Cu(PPh3)4]BF4
Reflux 0.114 grams (0.480 mmol) of Cu(BF4)2·NH2O and 0.755 grams (2.88 mmol) of triphenylphosphine in
absolute ethanol (200 proof) (15 mL) until the color changes from blue to white. This change can happen
fast; be sure to allow the solution to reflux ~10 min after observing the color change.
1.
After the reaction mixture is allowed to cool, isolate the complex by vacuum filtration using a glass fritted
filter. Note that an ice bath may be necessary for full precipitation.
2.
3. Determine the mass of the product. The precipitate contains [Cu(PPH3)4]BF4 as well as some co-
precipitated PPH3.
B. Preparation of 2,9-Dimethyl-1,10-phenanthroline-bis(triphenylphosphine)copper(1) tetrafluoroborate
Add 0.500 grams (0.417 mmol) of the [Cu(PPH3)4]BF4 synthesized in Part A to a 250-mL round bottom flask
with approximately 100 ml of anhydrous diethylether.
1.
In a separate beaker, dissolve 0.0723 grams (0.347 mmol) of 2,9-dimethyl-1,10-phenanthroline (DMP) in
approximately 20 mL of diethylether. If the DMP does not dissolve fully in the ether, add a minimal
2.
amount of ethanol to aid in the dissolution.
3. Slowly add the DMP solution to the copper solution over a period of 30 minutes. Allow the solution to stir
for approximately one hour following the addition of DMP.
4. The
progress of the reaction can be followed by the use of a UV-handlamp. The triphenylphosphine will
glow purple. As the mixed ligand complex forms the solution will glow an orange or yellow color.
5. Isolate the solid product via vacuum filtration.
6.
Wash the product repeatedly with ether to remove any excess triphenylphosphine still present.
7. Weigh the [Cu(DMP)(PPH3)2]BF4 obtained and calculate the percent yield.
lts fron
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