Antimony trifluoride

Antimony trifluoride, Sbp3, m.p. 292°C, sublimes319 C(Sb203 in HFsolution). Forms complex ions, e.g. [SbFJ". Widely used as a fairly mild fluorinating agent. 

Alkoxy fluorides are prepared using acetyl fluoride. Alternatively, antimony trifluoride can be used to replace one alkoxyl by fluorine (58) ... 

Antimony Trifluoride. Antimony(Ill) fluoride [7783-56-4] SbF, is a white, crystalline, orthorhombic soHd vapor pressure at the mp, 26.34... 

Parameter Antimony trifluoride Antimony trichloride Antimony tribromide Antimony ttiiodide Antimony pentafluoride Antimony pentachloride... 

In the presence of excess fluoride, antimony trifluoride forms numerous types of complex ions, eg, SbF , SbF , Sb4F 23, and Sb2F 2 but SbF is unknown (26). 

In the presence of catalysts, trichloroethylene is readily chlorinated to pentachloro- and hexachloroethane. Bromination yields l,2-dibromo-l,l,2-trichloroethane [13749-38-7]. The analogous iodine derivative has not been reported. Fluorination with hydrogen fluoride in the presence of antimony trifluoride produces 2-chloro-l,l,l-trifluoroethane [75-88-7] (8). Elemental fluorine gives a mixture of chlorofluoro derivatives of ethane, ethylene, and butane. 

Antimony trifluoride [7783-56-4] M 178.8, m 292 . Crystd from MeOH to remove oxide and oxyfluoride, then sublimed under vacuum in an aluminium cup on to a water-cooled copper condenser [Woolf J Chem Soc 279 1955]. 

Antlu acite hidustries hic., 217, 218 Antlu aqumones, 17 Antibiotics S.p.A., 180 Antimony, 18 Antimony lactate, 18 Antimony pentachloride, 18 Antimony pentafluoride, 18 Antimony potassium tailrate, 18 Antimony tribromide, 18 Antimony trichloride, 18 Antimony trifluoride, 18 Antimony trioxide, 18 AntimycinA, 19 Antofagasta Pic, 206 ANTU, 19 ANWILS. A., 197 APAChic., 218... 

A one-pot synthesis of alkyl perfluoroalkyl ketones has been developed. Phosphoranes, generated in situ, are acylated with a perfluoroacyl anhydnde, and the resultmg phosphonium salts are hydrolyzed with alkali [4S (equation 48) Hydrolysis of a carbon-sulfur bond in 2-chloro-2,4,4-trifluoro-1,3-dithietane-S-trioxide, which can be obtained from 2,2,4,4-tetrachloro-l,3-dithietane by fluor-mation with antimony trifluoride followed by selective oxidations, opens the nng to produce 2-chloro-1,1,2-trifluorodimethyl sulfone [49] (equation 49)... 

N P Cl (NEt2) 2 (as monitored by F nmr and glc) with antimony trifluoride gives the cis non-geminal difluoride while the use of potassium fluorosulfate gives the cis geminal difluoride. The tetrafluoro derivative, cis-2,4-N P F (NEt, ) can be obtained from... 

Apparatus. The generator employed is shown in fig. 10. There are six important points. (1) The column. <4 is designed so that throttling is avoided it is at least 2 ft. long and surmounted by a reflux doublesurface water-condenser B. (2) A Perkin triangle (air-cooled), inserted between the down-condenser and the traps, enables any phosphorus oxychloride which distils to be removed. (3) It is convenient to have three traps, viz. C, ice and salt D, acetone and carbon dioxide E, liquid air. (4) The intermittent addition of the solid antimony trifluoride presents a problem. The mechanical solid feed... 

Procedure. Finely powdered antimony trifluoride is placed in the reservoir of the feed. Phosphorus oxychloride and then antimony pentachloride are placed in the reaction vessel. The temperature of the bath is maintained, thermostatically, at 75° and the pressure kept at 190-200 mm., and the antimony trifluoride is then added slowly from the feed. The distillates in the traps are united and fractionated. The distillate, up to b.p. 90°/760 mm., is collected and carefully refractionated, giving pure phosphorus oxydichlorofluoride, b.p. 54° (20 per cent yield). 

In view of the high toxicity of (II), it seemed that the sulphur analogue, dimethylaminosulphonyl fluoride (VI), might be of some interest. We therefore studied the fluorination of dimethylaminosulphonyl chloride. The reaction with potassium fluoride was incomplete, and that with zinc fluoride unsatisfactory, but that with antimony trifluoride using benzene as a solvent proved to be very satisfactory, and an 80 per cent yield of (VI) was obtained. Physiological examination showed that (VI) caused no irritation when small animals were exposed to a concentration of 1 mg./l. for 10 min., and no deaths took place. With the sulphonyl chloride at the same concentration, lacrimation and nasal irritation were caused no deaths were recorded, and all the animals recovered almost immediately on being removed from the chamber. 

An attempt to prepare 1 -bromo-2-fluoroethane by the partial fluorination of ethylene dibromide by means of antimony trifluoride was not very successful. The compound was best prepared by the action of phosphorus tribromide on F.E.A. The compound was relatively non-toxic and the bromine atom rather unreactive, but considerably more reactive than the chlorine atom in chlorofluoroethane. For example, bromofluoroethane was readily converted by means of potassium thiocyanate into 2-fluoroethyl thiocyanate. As a lethal inhalant the toxicity of the thiocyanate was inferior to that of M.F.A. Toxicity by injection, however, appeared to be higher. 

Several methods are available for the synthesis of CFsSBr. Either CF2BrSBr is fluorinated at 100°C with antimony trifluoride (186) or CFsSCl is reacted with bromine cyanide over activated carbon at 70°C (86). Apart from that it is obtained always contaminated with CFsSSCFj in the reaction between Hg(SCF8)2 and bromine (31) these compounds react at 0°C to give a mixture composed of 56% CFsSBr and 45% CFjSSCFs. 

Sb is oxidized by nitric acid, forming a gelatinous precipitate of bydrated antimony pentoxide. It does not react with cold dilute sulfuric acid. However, reaction occurs in bot concentrated acid an oxysulfate of indefinite composition and low acid-solubdity is formed. It reacts with bydrofluoric acid to form soluble antimony trifluoride and pentafluoride. Hydrochloric acid in the absence of air does not readily attack tbe metal however, finely divided antimony reacts with hot concentrated acid forming chloride salt. 

It may also be prepared from antimony trifluoride and fluorine, or by treating antimony pentaoxide with aqueous hydrofluoric acid and evaporing water. 

Antimony trioxide is an amphoteric oxide, exhibiting both acidic and basic behavior. It dissolves in strong acids forming antimony salts e.g., reacts with aqueous hydrofluoric acid to form antimony trifluoride, SbFs. It reacts with strong alkalies to form antimonites, such as sodium or potassium anti-monites, NasSbOs or K38b03 ... 

Reactions with antimony trifluoride, SbFs in the presence of antimony pen-tachloride, SbCls, form mixed halides of compositions GeClsF, GeCl3F2, GeCl2F2, and GeClFs. 

Antimony trifluoride, 16 181 preparation of, 7 14-15 solubility of, 7 6-7 Antimony trifluoroacetates, 17 12, 13 Antiperspirants, 36 16 Anti-Stokes emission, 35 342-343 Antitumor agents DNA and RNA cleavers, 45 252 phosphazotrihalides as, 14 90, 91... 

Fluorophosphites are prepared by a two step sequence. The initial step is the reaction of phenolic materials with phosphorus trichloride to prepare a chlorophosphite intermediate. The chlorophosphite is then treated with a fluoride source to convert the chloro- intermediate into the desired fluorophosphite product. Many different fluoride sources have been described in the literature including anhydrous hydrogen fluoride, anhydrous potassium fluoride, and antimony trifluoride. While any of these fluoride sources can be used successfully, we have found that antimony trifluoride (10) works well for small scale, lab preparations. 

A number of routes to thiocarbonyl fluoride that do not involve tetrafluoro-dithietane have been developed. In one (50), phosgene is chlorinated to give tri-chlorosulfenyl chloride, which is converted to chlorodifluorosulfenyi chloride by reaction with antimony trifluoride, and the fluorinated compound is then dehalogenated by reaction with tin. 

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