Solved by verified expert:Synthesis of KBArF
4 and FcBArF
4read Guidelines1-write a lab report Conclusions only 2- answer the questions 3- Table of Contents Graphic (TOC)use the template and read every thing Sample % yield calculation I will provide my notes
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Chem 410 Lab Report Grading Rubric for Conclusions Only
No Title or
Missing a title or
All author contact
only a generic
a lack of
about how to
points are drawn,
but many are
indicating a lack
been drawn, but
been drawn, but
one major point is
been drawn, but
two minor points
been drawn, but a
minor point is
been drawn, could
be better stated
conclusions have been
clearly made, student
Five or more
Three or more
Missing more than
two items in SI
Incorrect Table of
Contents or missing
one item in SI
All SI and Table of
notebook pages in
No TOC Graphic
TOC Graphic can’t
be easily read (not
the correct size)
TOC Graphic is
missing a key result
TITLE (Word Style “BA_Title”). The title should accurately,
clearly, and concisely reflect the emphasis and content of the paper.
The title must be brief and grammatically correct. Do NOT delete
the space above the title.
AUTHOR NAMES (Word Style “BB_Author_Name”). Include in the byline all those who have made
substantial contributions to the work, even if the paper was actually written by only one person. Use
first names, initials, and surnames (e.g., John R. Smith) or first initials, second names, and surnames
(e.g., J. Robert Smith). Do not use only initials with surnames (e.g., J. R. Smith) because this causes indexing and retrieval difficulties and interferes with unique identification of an author. Do not include
professional or official titles or academic degrees. At least one author must be designated with an asterisk as the author to whom correspondence should be addressed.
AUTHOR ADDRESS (Word Style “BC_Author_Address”). The affiliation should be the institution where the work was
conducted. If the present address of an author differs from that at which the work was done, indicate with a symbol and give
the Present Address under Author Information. If more than one address, use symbols to match author names to address(es).
Submitted: [Enter submission date]
TEXT (Word Style “TA_Main_Text”). For full instructions,
please see the journal’s Instructions for Authors. Do not modify
the font in this or any other section, as doing so will not give an
accurate estimate of the formatting for publication and final length
of the paper.
ANSWERS TO QUESTIONS
Word Style “Section_Content”). A listing of the contents of each
file supplied as Supporting Information should be included. For instructions on what should be included in the Supporting Information, refer to the Chem 410 syllabus.
(Word Style “Section_Content”). Give contact information for the
author(s) to whom correspondence should be addressed.
(Word Style “TF_References_Section”). References are placed at the
end of the manuscript. Authors are responsible for the accuracy and completeness of all references. Examples of the recommended formats for the
various reference types can be found at http://pubs.acs.org/page/4authors/index.html. Detailed information on reference style can be found in
The ACS Style Guide, available from Oxford Press.
Table of Contents Graphic (TOC)
Chem 410 (Spring 2019)
Experiment 7: Synthesis of KBArF4 and Ferrocenium BArF4
Time Required: Four Three Hour Laboratory Periods
Lab Period 1: Grignard Reaction
To a 500 mL three-necked flask fitted with two glass stoppers (or rubber septa),
and a gas adaptor add magnesium turnings (3.00 g, 123.4 mmol). Purge the reaction flask
of oxygen. Fit an addition funnel and a reflux condenser. To the addition funnel, add 100
mL of degassed THF followed by the addition of 1,2 dibromoethane (1.0 mL). If no
reaction was observed after several minutes gently heat the reaction flask with a heat
gun to initiate the reaction.
Slowly add (over 35 minutes) a solution of 3,5-
bis(trifluoromethyl)-bromobenzene (8.50 mL, 49.3 mmol) in 40 mL degassed THF. The
solution should initially turn dark pink, and after all of the 3,5-bis(trifluoromethyl)bromobenzene is added, it may be a dark brown color. After the addition of the 3,5bis(trifluoromethyl)-bromobenzene is complete, the reaction solution should be refluxed
for an additional 30 min, heating itself. KBF4 (1.0 g, 7.94 mmol) was quickly added as a
solid under a stream of N2. The mixture then was stirred for 48 h at 23 °C (under N2). This
is a good place to stop for the day. Remove the condenser and the addition funnel and
replace with a stopper, and be sure to label your reaction flask.
Lab Periods 2 & 3: Purification of KBArF4
To the reaction mixture add a solution of K2CO3 (16.6 g) and KHCO3 in DI water
(200 mL), stir for ~15 min, and filter out any unreacted Mg. Using a separatory funnel,
extract the aqueous layer with ether (3 x 50 mL) and then dry the combined ether
fractions over MgSO4. Filter off the MgSO4, and remove under vacuum by placing the
flask on a rotary evaporator. The resulting product should be a dark brown oil. Seal the
flask containing the brown oil with a septum and parafilm, and clamp the flask to a
support beam in your hood.
The flask containing the dark brown oil should be secured to the Schlenk line. Place
a hot water bath (using a crystallization dish on top of the hot plate), heating the bath
until the water is boiling. Then immerse the flask containing the dark brown oil in the hot
water bath, and remove any residual solvent. After 30-40 minutes, a light brown powder
should start to form. Wash the resulting solid with cold methylene chloride to remove any
discoloration. Decant off the supernatant liquid, and filter the product using vacuum
filtration. Place the resulting product in a vial, sealed with your name. Prepare a NMR
sample in acetone-d6.
Ref: Yakelis, N. A.; Bergman, R. G. Organometallics 2005, 24, 3579-3581.
Lab Period 4: Synthesis and Purification of FcBArF4
Cp2FePF6 (0.153 g, 0.57 mmol) dissolved in CH2Cl2 (60 ml) was added to KBArF4
(0.50 g, 0.57 mmol) and the mixture was heated under reflux for 30 min. The solvent was
removed reduced pressure and the product was extracted with diethyl ether. The diethyl
ether was concentrated in vacuum to ca. 10 ml. Pentane (70 ml) was added and the blue
precipitate which formed was filtered, washed with pentane and then dried under
reduced pressure. The solid was recrystallised by slow diffusion of pentane into a
concentrated dichloromethane solution. After 24 hours the blue crystals were washed
with pentane and dried under reduced pressure.
Ref: Chavez, I.; Alvarez-Carena, A.; Molins, E.; Roig, A.; Maniukiewicz, W.; Arancibia, A.;
Arancibia, V.; Brand, H.; Manuel Manriquez, J. J. Organomet. Chem. 2000, 601, 126-132.
Chem 410 Lab Report Guidelines for
Experiment #7 – Synthesis of KBArF4 and FcBArF4
Please use the lab report templates available on Blackboard prepare a report based on your
assigned section (please see table below).
Lab Report Section Assignment
Questions to be Answered:
1) NaBArF4 ($146.50/250 mg from Aldrich) is a much cheaper reagent than KBArF4
($1,521/500 mg from Aldrich). The synthesis of NaBArF4, by a procedure similar to
KBArF4, generates NaBArF4•2.6 H2O (Organometallics, 2005, 24 (14), pp 3579–3581),
whereas the potassium salt is anhydrous. Discuss the advantages and disadvantages of
using NaBArF4 vs. KBArF4 in catalytic reactions?
2) Generation of the [BArF4]− required the use of a Grignard reagent. Discuss this reaction
and why THF was used as a solvent.
3) Discuss why a Griganrd reagent as opposed to a lithium reagent is used to generate the
4) What happened to the ferrocenium salt upon addition of KBArF4?
5) Discuss the characteristics of [BArF4]− salts. Why are these characteristics desired?
Data to be included in Supporting Information:
1) Cover page with Table of Contents
2) 1H, 11B, and 19F NMR spectra of KBarF4 and FcBArF4 in acetone-d6
3) Sample % yield calculation
4) Carbon copies from lab notebook
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