Chemical Science,
Journal Year:
2023,
Volume and Issue:
14(16), P. 4230 - 4247
Published: Jan. 1, 2023
This
review
explores
the
benefits
of
flow
chemistry
and
dispels
notion
that
it
is
a
mysterious
“black
box”,
demonstrating
how
can
push
boundaries
organic
synthesis
through
understanding
its
governing
principles.
Organic Process Research & Development,
Journal Year:
2024,
Volume and Issue:
28(2), P. 338 - 366
Published: Jan. 18, 2024
This
review
summarizes
examples
of
organic
electrosynthesis
from
the
peer-reviewed
literature
2000
to
2023
that
have
been
conducted
on
scales
20
g
or
above.
A
significant
portion
these
were
a
≤100
scale,
while
detailed
reports
kilogram-scale
remain
scarce
in
pharmaceutical
industry.
In
addition
chemical
transformation,
this
also
highlights
type
reactor
used
and
projected
productivity
metric
as
ways
compare
different
reports.
The
selected
scale-ups
described
herein
illustrate
remaining
challenges
currently
preventing
routine
use
large-scale
Angewandte Chemie International Edition,
Journal Year:
2023,
Volume and Issue:
62(15)
Published: Feb. 4, 2023
Interest
in
deuterated
active
pharmaceutical
ingredients
(APIs)
is
increasing
as
deuteration
holds
promise
for
kinetic
isotope
effect
(KIE)
regulated
fine-tuning
of
API
performance.
Moreover,
deuterium
labeling
frequently
carried
out
to
study
organic
and
bioorganic
reaction
mechanisms
facilitate
complex
target
synthesis.
As
such,
methods
highly
selective
molecules
are
desirable.
Herein,
we
present
an
electrochemical
method
the
deuterodehalogenation
benzylic
halides
via
a
radical-polar
crossover
mechanism,
using
inexpensive
oxide
(D
Journal of the American Chemical Society,
Journal Year:
2024,
Volume and Issue:
146(31), P. 21960 - 21967
Published: July 23, 2024
Oxygen-atom
transfer
reactions
are
a
prominent
class
of
synthetic
redox
that
often
use
high-energy
oxygen-atom
donor
reagents.
Electrochemical
methods
can
bypass
these
reagents
by
using
water
as
the
source
oxygen
atoms
through
pathways
involving
direct
or
indirect
(mediated)
electrolysis.
Here,
manganese
porphyrins
and
related
mediators
shown
to
be
effective
molecular
electrocatalysts
for
selective
oxidation
thioethers
sulfoxides,
without
overoxidation
sulfone.
The
proceed
proton-coupled
Mn
Organic Process Research & Development,
Journal Year:
2024,
Volume and Issue:
28(5), P. 1964 - 1970
Published: March 13, 2024
Although
continuous
flow
synthesis
using
microtubing
reactors
has
provided
a
wealth
of
opportunities
for
homogeneous
photochemical
and
proven
particularly
beneficial
in
scaling
up
processes,
employing
technology
to
scale
heterogeneous
photoreactions
is
challenging
due
the
issues
including
handling
solids,
poor
light
penetration,
commonly
lengthy
reaction
time.
Here
we
present
solution
these
by
changing
mode
high-speed
circulation
mode.
The
high
rate
set
reactor
overcomes
solid
sedimentation
prevent
clogging
improve
mixing
efficiency.
We
successfully
conducted
100
g-scale
C–N
C–S
cross-couplings
photocatalyst
nickel
catalyst
that
significantly
outperformed
conventional
batch
reactors.
was
recycled
reused
10
times
achieve
kilogram-scale
without
obvious
deactivation.
Semicontinuous
production
achieved
via
automated
feeding
collection,
photopromoted
gas/liquid/solid
three-phase
trifluoromethylation
employed.
A
amount
starting
material
transformed,
resulting
43.2%
yield
trifluridine.
Our
study
suggests
with
speed
will
become
crucial
tool
synthetic
chemist's
toolbox
because
its
simple
infrastructure,
ease
operation
automation,
significant
efficiency
improvement
compared
reactors,
scalability,
improved
safety,
tolerance
solids.
Organic Process Research & Development,
Journal Year:
2025,
Volume and Issue:
unknown
Published: Jan. 7, 2025
A
scalable
electrochemical
process
to
synthesize
iminophosphorane
ligands
is
reported.
The
application
of
these
iminophosphoranes
was
recently
reported
in
Ni-catalyzed
cross-electrophile
and
C–N
cross-couplings.
use
parallel
plate
flow
reactors
enables
the
synthesis
on
a
multigram
scale,
with
selected
examples
up
0.6
kg
scale.
Direct
crystallization
from
end
reaction
mixture
for
provides
facile
isolation
processes.
This
article
also
details
improvements
our
capabilities
across
scales,
including
addressing
material
compatibility
issues,
increasing
accessible
range
rates,
integration
analytical
technology
tools.
Organic Process Research & Development,
Journal Year:
2023,
Volume and Issue:
27(11), P. 2072 - 2081
Published: Oct. 11, 2023
Technology
for
the
rapid
scale-up
of
synthetic
organic
electrochemistry
from
milligrams
to
multigrams
or
multi-100
g
quantities
is
highly
desirable.
Traditional
parallel
plate
flow
electrolysis
cells
can
produce
large
material,
but
transfer
batch
this
technology
requires
reoptimization
reaction
conditions
and
fully
homogeneous
mixtures.
Moreover,
single-pass
processing
often
difficult
accomplish
due
gas
generation
low
rates
typically
used
in
continuous
mode.
Herein
we
present
a
novel
reactor
design,
based
on
rotating
cylinder
electrode
concept,
that
enables
seamless
scale
up
small
experimentation
gram
even
multikilogram
per
day
quantities.
The
device
operate
mode,
it
able
easily
process
slurries
without
clogging
system
fouling
electrodes.
Continuous
operation
also
demonstrated
using
three
reactors
series
act
as
stirred
electrochemical
cascade,
providing
kilogram
productivities
single
pass.
Chemistry - A European Journal,
Journal Year:
2023,
Volume and Issue:
29(18)
Published: Jan. 3, 2023
Alternating
current
(AC)
electrolysis
is
receiving
increased
interest
as
a
versatile
tool
for
mild
and
selective
electrochemical
transformations.
This
work
demonstrates
that
AC
can
enable
the
concept
of
stirring-free
reactor
where
periodic
switch
electrode
polarity,
inherent
to
AC,
provides
uniform
across
whole
volume
reactor.
Such
design
implies
straightforward
approach
scaling
up
electrosynthesis.
was
demonstrated
on
range
transformations
performed
in
three
different
RVC-packed
reactors
50-mmol
scale.
Redox-neutral,
oxidative,
reductive
processes
were
successfully
implemented
using
suggested
applicable
frequency
ranges
further
investigated
types
reactions.
The
advantages
AC-enabled
-
such
absence
stirring
maximized
surface
area
electrodes
provide
possibility
its
universal
application
both
small-scale
screening
experimentation
large-scale
preparative
electrosynthesis
without
significant
optimization
needed
between.
