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Flash Communication : A Glovebox-Friendly Synthesis of [CrCl3(THF)3] from CrCl2 and Trityl Chloride

Chandran, Aswin LU and Reinholdt, Anders LU (2026) In Organometallics 45(11). p.1198-1202
Abstract

mer-[CrCl3(THF)3] is a useful and labile precursor for Cr(III) organometallic chemistry, but the commercial material is costly and sometimes poorly defined, whereas existing synthetic routes to the complex rely on corrosive reagents, prolonged reaction times, or elaborate experimental setups which are impractical for glovebox work. Herein we present a facile, mild, and glovebox-friendly synthesis of mer-[CrCl3(THF)3] as purple crystals from CrCl2 using solid trityl chloride as a chlorinating agent in THF. The reaction proceeds in 2.5 h at 75 °C or overnight at room temperature, directly yielding crystalline mer-[CrCl3(THF)3] in 70–84% yield with minimal workup;... (More)

mer-[CrCl3(THF)3] is a useful and labile precursor for Cr(III) organometallic chemistry, but the commercial material is costly and sometimes poorly defined, whereas existing synthetic routes to the complex rely on corrosive reagents, prolonged reaction times, or elaborate experimental setups which are impractical for glovebox work. Herein we present a facile, mild, and glovebox-friendly synthesis of mer-[CrCl3(THF)3] as purple crystals from CrCl2 using solid trityl chloride as a chlorinating agent in THF. The reaction proceeds in 2.5 h at 75 °C or overnight at room temperature, directly yielding crystalline mer-[CrCl3(THF)3] in 70–84% yield with minimal workup; the only organic byproduct is Gomberg’s dimer, Ph3CC6H5CPh2, which is readily removed by hexane washings. This operationally simple method avoids corrosive, toxic, and volatile reagents, minimizes waste, and provides reliable and ready access to mer-[CrCl3(THF)3]. The THF adduct undergoes a clean ligand substitution reaction with Na(pyrNdipp) to afford the structurally characterized Cr(III) complex [Cr(pyrNdipp)2Cl(THF)], illustrating the synthetic utility of the material.

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publishing date
type
Contribution to journal
publication status
published
subject
in
Organometallics
volume
45
issue
11
pages
5 pages
publisher
The American Chemical Society (ACS)
external identifiers
  • scopus:105040908750
ISSN
0276-7333
DOI
10.1021/acs.organomet.6c00088
language
English
LU publication?
yes
id
42b66947-1dd5-46e0-b53e-7613b9395cdd
date added to LUP
2026-08-28 12:47:09
date last changed
2026-08-28 12:47:22
@article{42b66947-1dd5-46e0-b53e-7613b9395cdd,
  abstract     = {{<p>mer-[CrCl<sub>3</sub>(THF)<sub>3</sub>] is a useful and labile precursor for Cr(III) organometallic chemistry, but the commercial material is costly and sometimes poorly defined, whereas existing synthetic routes to the complex rely on corrosive reagents, prolonged reaction times, or elaborate experimental setups which are impractical for glovebox work. Herein we present a facile, mild, and glovebox-friendly synthesis of mer-[CrCl<sub>3</sub>(THF)<sub>3</sub>] as purple crystals from CrCl<sub>2</sub> using solid trityl chloride as a chlorinating agent in THF. The reaction proceeds in 2.5 h at 75 °C or overnight at room temperature, directly yielding crystalline mer-[CrCl<sub>3</sub>(THF)<sub>3</sub>] in 70–84% yield with minimal workup; the only organic byproduct is Gomberg’s dimer, Ph<sub>3</sub>CC<sub>6</sub>H<sub>5</sub>CPh<sub>2</sub>, which is readily removed by hexane washings. This operationally simple method avoids corrosive, toxic, and volatile reagents, minimizes waste, and provides reliable and ready access to mer-[CrCl<sub>3</sub>(THF)<sub>3</sub>]. The THF adduct undergoes a clean ligand substitution reaction with Na(pyrNdipp) to afford the structurally characterized Cr(III) complex [Cr(pyrNdipp)<sub>2</sub>Cl(THF)], illustrating the synthetic utility of the material.</p>}},
  author       = {{Chandran, Aswin and Reinholdt, Anders}},
  issn         = {{0276-7333}},
  language     = {{eng}},
  number       = {{11}},
  pages        = {{1198--1202}},
  publisher    = {{The American Chemical Society (ACS)}},
  series       = {{Organometallics}},
  title        = {{Flash Communication : A Glovebox-Friendly Synthesis of [CrCl<sub>3</sub>(THF)<sub>3</sub>] from CrCl<sub>2</sub> and Trityl Chloride}},
  url          = {{http://dx.doi.org/10.1021/acs.organomet.6c00088}},
  doi          = {{10.1021/acs.organomet.6c00088}},
  volume       = {{45}},
  year         = {{2026}},
}