homogeneous catalysis fluorescent dyes

12
Homogeneous Catalysis Fluorescent Dyes 1 Please contact: Prof. Dr. Herbert Plenio, Organometallic Chemistry, Alarich-Weiss-Str. 12, TU Darmstadt, 64287 Darmstadt, Germany, [email protected] Better Tools for the efficient synthesis of Organic Molecules and Polymers Understanding the mechanism Using Fluorescent Dyes to understand Homogenous Catalysis

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Page 1: Homogeneous Catalysis Fluorescent Dyes

Homogeneous Catalysis

Fluorescent Dyes

1

Please contact: Prof. Dr. Herbert Plenio, Organometallic Chemistry, Alarich-Weiss-Str. 12,

TU Darmstadt, 64287 Darmstadt, Germany,

[email protected]

• Better Tools for the efficient synthesis of Organic Molecules and Polymers

• Understanding the mechanism

• Using Fluorescent Dyes to understand Homogenous Catalysis

Page 2: Homogeneous Catalysis Fluorescent Dyes

Better Tools for the Conversion of

Molecules

RESEARCH TOPICS

superior synthetic tools =

Development of new catalysts

better synthesis =

new approaches for the synthesis

of organic molecules and polymers

Mechanistic understanding =

mechanistic studies of transition-metal

catalyzed transformations

www.lego.com

Herbert Plenio

2

Page 3: Homogeneous Catalysis Fluorescent Dyes

fast and low-loading

RCM catalysis

3

100 ppm 88%

100 ppm 89%

15 ppm 91%

50 ppm 89% P. Kos, R. Savka, H. Plenio, Adv. Synth. Catal. 2013, 355, 439

http://onlinelibrary.wiley.com/doi/10.1002/adsc.201200956/abstract

Page 4: Homogeneous Catalysis Fluorescent Dyes

Research Topic: Renewables

Ethenolysis of natural rubber and tire rubber

n

natural rubber

cis-Polyisoprene

Hevea brasiliensis

n

[Ru] -catalyst

++

+ethene

On the ethenolysis of end-of-life tire granulates

S. Wolf, H. Plenio, Green Chem. 2013, 15, 31; http://dx.doi.org/10.1039/C2GC36417D

The ethenolysis of natural rubber or tire

rubber granulate leads to the depoly-

merization of the polymer, resulting in the

facile formation of small terpenes, which

might be suitable for the synthesis of

fragrances.

Herbert Plenio

4

Page 5: Homogeneous Catalysis Fluorescent Dyes

Gold-catalyzed Hydration of Alkynes

5

M. Heidrich, M. Bergmann, D. Müller-Borges, H. Plenio, Adv. Synth. Catal. 2018, 360, 3572,

https://onlinelibrary.wiley.com/doi/full/10.1002/adsc.201800605

Page 6: Homogeneous Catalysis Fluorescent Dyes

organic solubles obtained after

ethenolysis of ELT powder

6

[Ru]

7 barethenetoluene

80 oC

fest

flüssig

10 g of ELT yield up to 5 g of organic solubles

10 g of ELT require 0.04 g of ruthenium complex

Page 7: Homogeneous Catalysis Fluorescent Dyes

Understanding the mechanism

7.

On the Mechanism of the Initiation Reaction in Grubbs-Hoveyda Complexes

V. Thiel, M. Hendann, K. J. Wannowius, H. Plenio, J. Am. Chem. Soc. 2012, 134, 1104; ACS Catal.

2019, 9, 951 https://doi.org/10.1021/acscatal.8b03445

Progress in catalysis critically relies on detailed mechanistic

understanding. The development of olefin metathesis over

the last decades from ill-defined, low-activity catalysts to

powerful synthetic tools is an excellent example for this.

Herbert Plenio

Page 8: Homogeneous Catalysis Fluorescent Dyes

Understanding the Mechanism

350 400 450 500 5500.0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

absorb

ance

nm]

0 50 100 150 200 250 300 350 4000.0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

1.0

absorbance at 377 nm

absorb

ance

time (s)

equaton y = A1*exp(-x/t1) + y0

R^2 0.99995

value error

y0 0.18493 1.77929E-4

A1 0.71613 0.00108

t1 42.28923 0.09367

0.0 0.5 1.0 1.5 2.0 2.50.00

0.02

0.04

0.06

0.08

kobs (

s-1)

[BuVE] (mol·L-1)

kobs = a·[olefin]/(1+b·[olefin]) + c·[olefin]

M CH2

MM

M

[2+2]

[2+2]

The activation of precatalysts leads to the generation of a

catalytically active species. Analysis of initiation kinetics

with time-dependent spectroscopic techniques provides

a clearer picture of the elementary steps of precatalyst

activation.

8

Page 9: Homogeneous Catalysis Fluorescent Dyes

Bodipy-tagged Crabtree Catalysts

= 0.049 = 0.51

P. Kos, H. Plenio, Angew. Chem. Int. Ed. 2015, 54, 13293-13296http://onlinelibrary.wiley.com/doi/10.1002/anie.201506918/abstract

air containing H2

impregnated with complex filter paper strip

0 1 1004H2, vol %:

Paper strips for

H2 detectionH2

Page 10: Homogeneous Catalysis Fluorescent Dyes

FRET for the detection of

dimeric Gold Catalysis

10

O. Halter, H. Plenio, Chem. Commun. 2017, 53, 12461,

http://pubs.rsc.org/en/content/articlepdf/2017/cc/c7cc07018g

Page 11: Homogeneous Catalysis Fluorescent Dyes

Detecting CO a few nanomols of CO

0 4 8 12 16 200

5

10

15

20

em

issi

on

/ a.u.

time / s

+10 eq CO

Ir

Rh

0 100 200 300 400 5000

10

20

30

40

50

em

issio

n /

a.u.

time / s

+ 25 nmol CO

Ir

• 80-fold fluorescence increase for iridium complex

• Complete conversion in less than 4 s for Ir

• Detection of less than 1 nanomol of CO

Page 12: Homogeneous Catalysis Fluorescent Dyes

Observing Ethene Insertion in Olefin

Polymerization Catalyst

12O. Halter, J. Spielmann, Y. Kanai, H. Plenio, Organometallics 2019, 38, 2138,

https://doi.org/10.1021/acs.organomet.9b00130