Antimony V Chloride Reagent

Table 46. h.Rf-values of vitamin E and related com pcmnds and coloration toitk antimony(V)-chloride reagent (12—18 cm run in 40-60 min)... 

Dipping solution Mix 2 ml antimony(V) chloride with 8 ml carbon tetrachloride. Storage The reagent solution should always be freshly prepared. 

Reaction of 13C-labeled chloroform with this reagent for 3 hours at O C gives 13CHFC12 as the major product. Under modified conditions, when 13CHC13 is added to the fluorinating agent [4 g of solid antimony(III) fluoride and 4 g of liquid antimony(V) chloride] and is warmed to 40 °C, the volatile product that distills off at — 90°C is 13C-labeled chlorodifluoromethane (80% conversion).73... 

In the fluorination of l,l.l,3,3,3-hexafluoro-2-(trichloromethyl)propan-2-ol with antimony fluoride the product 12 or 13 obtained is dependent upon whether antimony(V) fluoride or antimony(III) fluoride/antimony(V) chloride is used as the fluorinating reagent." ... 

The complete replacement of the chlorine atoms in (trichloromethyl)benzene by fluorine to give (trifluoromethyl)bcnzene is possible under mild conditions. This transformation can be achieved with a variety of reagents with anhydrous hydrogen fluoride the reagent of choice due to cost and the lack of side reactions. "Substituted (trichloromethyl)benzenes are successfully transformed into the corresponding (trifluoronicthyl)benzenes 1-3 by hydrogen fluoride in the presence of a catalytic amount of antimony(V) chloride.A procedure is given for the formation of 1-(dichloromethyl)-2-(trifluoromethyl)benzene (4). ... 

Vitamin E compounds can be detected (about 20 /tg) as dark spots in UV light. They appear violet and detection is appreciably more sensitive (0.02 /tg) on layers that contain 0.02% Na-fluorescein. Moreover, these are visible in daylight as reddish spots (limit of detection 2 fig). The same effect is produced by spraying with fluorescein or dichlorofluorescein reagent. Nonspecific visualization procedures for tocopherols and tocotrienols are based on spraying with sulfuric acid, molybdophosphoric add, antimony(V) chloride, dipyridyl-iron reagent, nitric add, and copper(II) sulfate-phosphoric add [1-4]. 

Detection The less volatile tar bases can be detected on fluorescent layers (e. g., silica gel GF264)- Other possibilities are using the spray reagents listed for the amines, e. g., iodine solution (Rgt. No. 144), permanganate solution (Rgt. No. 200), antimony(V) chloride (Rgt. No. 18) or the modified Dragendorff reagent for alkaloids (Rgt. No. 98). 

Also using silica gel G layers, Bbaun [4, 5] has separated numerous plasticisers with methylene dichloride, after they had been extracted from the plastic material with benzene or ether (provided the polymer itself was not soluble). Antimony(V)chloride (Rgt. No. 18) is a generally applicable spray reagent it yields brown spots with most of the plasticisers after the plate is heated to 120° C. Phthalate esters can be detected in addition with resorcinol solution (Rgt. No. 218) and phosphate esters with a diazonium salt reagent (No, 238). 

The substances are detected by inspection of the layer in UV light or by spraying with reagents such as antimony(V)chloride (No. 18), tetracyanoethylene (No. 243) or formaldehyde-sulphuric acid (No. 125). 

Spray reagent Antimony(V) chloride -f chloroform or carbon... 

Oxides and peroxides can occur in many essential oils by a photochemical reaction. 1,8-Cineol and linalool monoxide can be readily separated on silica gel thin layers with 1-nitropropane-hexane (1 1, v/v), as the mobile phase.In this case, they have exhibited Rf values of 73 and 8, respectively. " Another pair of compounds, ascaridole and 1,8-cineol, can be easily separated on a silica gel layer, obtaining a value for chloroform as the mobile phase of 63 and 54, respectively. The antimony chloride reagent gives a gray color. The potassium iodide-acetic acid-starch test is usually better than ferrous thiocyanate. 

---