Girard P reagent

Girard reagent p< CjH CINjO, l-(2-hydrazino-2-axoeth-yDpyridinium chloride- Non-hygroscopic crystals from methanol, dec 200". Less soluhle in polar solvents than Girard reagent T. 

Water-soluble hydrazones are also provided by the Girard reagents P and T,524,929 which have proved their worth for separation of mixtures of natural products.930, 931 The condensation is usually effected in aqueous methanol buffered with acetate.524... 

Rat brain (100 mg) —> ethanol extraction anion-exchange column (Lipidex DEAP) —> NP-mini-column oxidation with cholesterol oxidase —> derivatization with Girard reagent P Bovine adrenal cell culture medium LLE (ethyl acetate)... 

Girard s reagent P , C5H5NCH2C0NHNH2 C1. In a 1-htre threenecked flask, equipped as in the previous preparation, place 200 ml. of absolute ethyl alcohol, 63 g. (64 -5 ml.) of pure anhydrous pyridine and 98 - 5 g. (84 5 ml.) of ethyl chloroacetate. Heat the mixture under reflux for 2-3 hours until the formation of the quaternary salt is complete acidify a small test-portion with dilute sulphuric acid it should dissolve completely and no odour of ethyl chloroacetate should be apparent. Cool the mixture in ice and salt. Replace the thermometer by a dropping funnel, and add a solution of 40 g. of 100 per cent, hydrazine hydrate in 60 ml. of absolute ethanol all at once. A vigorous exothermic reaction soon develops and is accompanied by vigorous effervescence. The pro duct separates almost immediately. When cold, filter with suction, wash... 

Fraction 3 showed two retention times (a) the same as that of cyclohexenol, and (b) the same as that of cyclohexenone the infrared spectrum showed strong absorption bands at 3350 cm. 1 (—OH) and 1680 cm."1 (C=0 conjugated). This was separated into two fractions by Girard s P reagent. The a-naphthylurethane derivative of cyclohexenol was not depressed, m.p., 154.5°-155.5°C. [literature value, 156°C. (22)]. 

Girard 8 reagent P to form a pyridinium salt. Positive ion FAB... 

We have also employed other derivatization techniques to selectively label other moieties such as carbonyls and applied these to the selective detection of steroids [119]. Girard s Reagent P reacts with the carbonyl-containing compounds according to Equation 5. 

Carbonyl-Free Methanol Add 5 g of Girard s Reagent P (Aldrich, or equivalent) and 0.2 mL of hydrochloric acid to 500 mL of methanol, and reflux for 2 h. Distill the refluxed methanol through a short Vigreux column, and store in tightly closed bottles. 

New complexes containing azo- and hydrazinato-derivatized Schiff base ligands298 375 continue to be used for the analytical determination of vanadium.376 The vanadium complex was characterized for the Schiff base derived from the condensation reaction of benzoyl acetone and Girard s reagent P.377 Azophenolates of mononuclear and mixed valence dinuclear species have been reported.378 Naphthanol- or quinolinol-derivatized ligands prefer to chelate iron over vanadium.379... 

The reagent is analogous to Girard reagents T and P and is prepared in the same way and used for isolation of a ketone from a mixture by conversion to a derivative extractible from ether with dilute hydrochloric acid. It is stated to be more easily purified than reagents T and P. 

Trimethylaminoacetohydrazide chloride Trimethylammonium acetyl hydrazide chloride Trimethylammonium chloride acethydrazide. Reacts with ketones to form water-soluble hydrazones. Used in the isolation of ketosteroids. Girard s reagent P [1126-58-5], used in the same way, is 1-(2-hydrazino-2-oxoethyl)pyridinium chloride. Crystals mp = 192° soluble in H2O, polar organic solvents, insoluble in non-polar organic solvents. 

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