Determination of Sodium Fluoroacetate in Dairy Powders by Liquid Chromatography-Tandem Mass Spectrometry: Single-Laboratory Validation, First Action 2015.02.

A single-laboratory validation (SLV) study was conducted for the determination of sodium fluoroacetate in dairy powders by LC-tandem MS (LC-MS/MS). Linearity of response was confirmed by analysis of samples fortified over the concentration range 0.10-100 μg/kg.

Amine-free approach toward N-toluenesulfonyl amidine construction: a phosphite-mediated Beckmann-like coupling of oximes and p-toluenesulfonyl azide.

Atom hopping: A chlorophosphite-mediated Beckmann ligation of oximes and p-toluenesulfonyl azide gives access to N-sulfonyl phosphoramidines in good to excellent yields. The reaction proceeds under exceptionally mild conditions and constitutes a bioorthogonal approach toward amidines by avoiding the use of amines and transition-metal catalysts. dmp-ol=3,3-dimethylpropanediol.

Cooperative titanocene and phosphine catalysis: accelerated C-X activation for the generation of reactive organometallics.

The study presented herein describes a reductive transmetalation approach toward the generation of Grignard and organozinc reagents mediated by a titanocene catalyst. This method enables the metalation of functionalized substrates without loss of functional group compatibility. Allyl zinc reagents and allyl, vinyl, and alkyl Grignard reagents were generated in situ and used in the addition to carbonyl substrates to provide the corresponding carbinols in yields up to 99%.

Organozinc generation via the titanium-catalyzed activation of alkyl halides.

A protocol for the generation of organozinc reagents via catalytic activation of alkyl halides is described herein. Subsequent nucleophilic addition to carbonyl derivatives provided the desired products in good to excellent yields (76-99%). Evidence suggests that titanocene dichloride catalyzes the formation of an organozinc species.