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Evolved RebH chlorinates indoles at C5, C6 or C7

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Mass-spectrometry-guided evolution of RebH produced variants that chlorinate tryptamine ortho, meta or para to the indole nitrogen without a synthetic directing group.

Source

Directed Evolution of RebH for Catalyst-Controlled Halogenation of Indole C-H Bonds

Andorfer MC, Park HJ, Vergara-Coll J, et al. · Chemical science · 2016

doi.org/10.1039/c5sc04680gRead the full paper ↗77 citationscc by

What they did

Authors screened error-prone and site-saturation libraries of RebH on deuterium-labeled tryptamines by MALDI/LC-MS, then characterised variants 0S, 8F and 10S for 7-, 6- and 5-chlorination including docking versus native tryptophan binding.

What they found

0S (N470S) raised 7-chlorination yield 2.5-fold at >99% selectivity. 8F reached 85% 6-selectivity and 11-fold more 6-chlorotryptamine than 7M. 8F/10S still select C6/C5 despite weak binding, not the innately reactive C2.

The limits

What it doesn't show

Docking poses are models; crystal structures of the evolved variants with tryptamine were not solved, so how mutations retune binding remains unproven.

Key terms

RebH
Flavin-dependent tryptophan 7-halogenase used as the evolution parent.
Catalyst-controlled C–H halogenation
Site selectivity set by the enzyme, not by a substrate directing group.
8F / 10S
Evolved variants selective for 6- and 5-chlorotryptamine, respectively.
MALDI-MS screen
High-throughput mass assay using deuterated probes to score isomer ratios.
HalA
Computed C–H chlorination barrier used to rank innate site reactivity.

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Native RebH prefers chlorination at:

Common questions

What native RebH site is preferred?

The 7-position of the indole.

What selectivities did 8F and 10S achieve?

Almost exclusive 6- and 5-chlorination, respectively.

Did they need a directing group on the substrate?

No—selectivity is catalyst-controlled.

How was 5 vs 6 distinguished?

Deuterium-substituted probes plus MS.

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