Skip to Content
Merck
  • Brønsted acidic ionic liquid accelerated halogenation of organic compounds with N-Halosuccinimides (NXS).

Brønsted acidic ionic liquid accelerated halogenation of organic compounds with N-Halosuccinimides (NXS).

Molecules (Basel, Switzerland) (2013-01-25)
Dejan Vražič, Marjan Jereb, Kenneth K Laali, Stojan Stavber
ABSTRACT

The Brønsted-acidic ionic liquid 1-methyl-3-(4-sulfobutyl)imidazolium triflate [BMIM(SO(3)H)][OTf] was demonstrated to act efficiently as solvent and catalyst for the halogenation of activated organic compounds with N-halosuccinimides (NXS) under mild conditions with short reaction times. Methyl aryl ketones were converted into α-halo and α,α-dihaloketones, depending on the quantity of NXS used. Ketones with activated aromatic rings were selectively halogenated, however in some cases mixtures of α-halogenated ketone and ring-halogenated ketones were obtained. Activated aromatics were regioselectively ring halogenated to give mono- and dihalo-substituted products. The [BMIM(SO(3)H)][OTf] ionic liquid (IL-A) was successfully reused eight times in a representative monohalogenation reaction with no noticeable decrease in efficiency. An effective halogenation scale-up in this IL is also presented. The reactivity trend and the observed chemo- and regioselectiivities point to an ET process in these IL-promoted halofunctionalization reactions.

MATERIALS
Product Number
Brand
Product Description

Supelco
Acetophenone, analytical standard
Sigma-Aldrich
Acetophenone, puriss. p.a., ≥99.0% (GC)
Sigma-Aldrich
Acetophenone, ≥98%, FG
Sigma-Aldrich
Acetophenone, ReagentPlus®, 99%
Supelco
Acetophenone solution, certified reference material, 2000 μg/mL in methylene chloride