© Division of Chemical Education • www.JCE.DivCHED.org • Vol. 86 No. 7 July 2009 • Journal of Chemical Education 853
In the Laboratory
Substitution reactions are valuable teaching tools in the un-
dergraduate classroom. hey teach students the fundamentals of
organic reactivity and provide the foundation for understanding
many organic reaction mechanisms. S
N
1 reactions are particu-
larly useful for imparting students with a solid understanding of
carbocations, including their stability, resonance, and ability to
rearrange. Despite the utility of these reactions for explaining
the basis of reactivity, there are few examples in the educational
literature.
Background
Experiments that demonstrate the use of an S
N
1 reaction
for the synthesis of ethers exist (1, 2). Procedures for the acid-
catalyzed ether formation of ethyl t-butyl ether (1) and Methyl
Diantilis, a fragrance (2), are available from this Journal. Al-
though these experiments provide options for implementing
a S
N
1 reaction, there are drawbacks to both procedures. he
ethyl t-butyl ether synthesis requires the use of sulfuric acid
and the isolation of the ether involves both a distillation and a
liquid–liquid extraction. he fragrance is available from vanillin
in two steps. However, the irst step is a sodium borohydride
reduction reaction of an aldehyde, which is oten addressed
much later than substitution reactions in the course curriculum.
In addition, the analysis of the fragrance involves both
1
H NMR
and IR spectroscopy, which is usually performed in the second
semester of the laboratory.
here are a number of experiments that look at the forma-
tion of carbocations to determine the stability of the carbo-
cation or the rate of formation of the carbocation (3–7). A
semi-empirical and DFT computational experiment has been
reported that looks at the dissociation of alkyl halides to show
the order of stability of alkyl substituted carbocations (3). he
analysis of the dissociation of alkyl halides is valuable in terms
of reinforcing the stability of cations, but there is no hands-on
synthesis involved in this laboratory. Many of the published
solvolysis experiments are designed to measure the rate of car-
bocation formation (4–7). hese are good experiments for a
physical chemistry laboratory, but they do not allow students
to experience the isolation of the solvolysis products, which is
an important part of the learning process.
Rationale
here is a lack of experiments available for the S
N
1 reaction
that meet the following criteria: short reaction times, easy prod-
uct isolation, easy product puriication, high yields, relatively
benign reagents (no strong acids or strong lachrymators), and
no competing reactions. Owing to the utility of S
N
1 reactions
in providing a strong foundation for understanding organic
reactivity, a new laboratory was developed that would allow
the students to apply the optimal conditions for a solvolysis
reaction. he reaction of bromodiphenylmethane is quick (7),
and it was anticipated that bromotriphenylmethane would un-
dergo reaction more readily and quickly, due to the additional
stability associated with a tertiary carbocation that is highly
resonance stabilized (8). In addition, bromodiphenylmethane is
a lachrymator whereas bromotriphenylmethane is not. Bromo-
triphenylmethane was chosen as a substrate because it dissoci-
ates quickly to generate a stable carbocation intermediate and
allows the reaction to occur in a reasonable time. In addition,
triphenylmethanol and many triphenylmethyl ethers are solids,
which would allow the students to isolate a product, determine
the melting point for product conirmation, and highlight the
solvolysis of a tertiary substrate.
he triphenylmethyl cation is well known for its stability.
It is commercially available from Sigma–Aldrich as the tetra-
luoroborate salt. One method for the generation of the highly
colored cation is the treatment of triphenylmethanol with a
strong acid, such as luoroboric acid or sulfuric acid (9). Also,
substituted triphenylmethyl cations are dyes that are used for
wool and silk (10), which provides relevance for this experience
to everyday life.
Experiment
Bromotriphenylmethane (1.6 mmol) 1 is added to acetone
then a large excess of water or the appropriate alcohol is added.
he reaction to generate triphenylmethanol 2 and the remaining
triphenylmethyl ethers is almost instantaneous.
Ph
Ph
Ph Br
Ph
Ph
Ph OR
H:
R =
2
Me: 3
Et: 4
1-Pr: 5
1-Bu: 6
1
ROH
he reaction to generate triphenylmethanol 2 and the remain-
ing triphenylmethyl ethers is almost instantaneous. he process
of monitoring the reaction by GC–MS shows that even ater
1 minute, no bromotriphenylmethane remains in the reaction
mixture. Product isolation is straightforward for triphenylmeth-
anol 2, triphenylmethyl methyl ether 3, and triphenylmethyl
ethyl ether 4 (9); the addition of the reaction solution to ice
causes the product to crystallize and precipitate from solution so
that it may be collected by suction iltration. he crude product
is recrystallized from 2-propanol. In the cases of the 1-propyl
ether 5 and 1-butyl ether 6, the product must be extracted from
the aqueous solution with dichloromethane and concentrated
to give a solid product.
A Flexible Solvolysis Experiment for the Undergraduate
Organic Laboratory
John J. Esteb, John R. Magers, LuAnne McNulty,* Paul Morgan, Kathryn Tindell, and Anne M. Wilson
Department of Chemistry, Butler University, Indianapolis, IN 46208; *lmcnulty@butler.edu