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A simplified method for the quantitative analysis of hyoscyamine hydrobromide or atropine in Belladonna Tincture USP is described. The procedure is based on the formation of an alkaloid-dye complex which can be extracted with an organic solvent and measured spectrophotometrically. The results obtained by this method compare favorably with those obtained by the USP method.

Chemistry Department, Rajasthan University, Jaipur-302004 Manuscript received 9 November 1976, accepted 2 April 1977 1, 3, 5, 2-Oxadiazaboroles of the types, R(HN)C =NOB - OR', └―――┘ R(HN)C =NOB - ON= C(R)NH—BON=C(NH)R, R(HN)C =NOB. Ph and └―――┘ └―――┘ └―――┘ [R(HN)C=NOB]2—O, (where R=Me, Et, Pr or Ph and R' =Et or Pri) └―――┘ have been synthesized from the reactions of alkylborates, phenylboronic acid or boric acid with amidoximes and characterized

Bis(1,3,5,2-oxadiazaborol-2-yloxy)tetrabutyldistannoxanes have been synthesized by the reaction of amidoxime, boric acid and dibutyltin oxide. A probable structure for the dimeric species has been proposed on the basis of molecular weight and IR spectral data.

A quantitative method for the assay of phenol in ointments is described. The procedure involves the formation of a blue indophenol by reacting phenol with 2,6-dibromoquinone-4-chloroimide which can be measured spectrophotometrically. The method is accurate, and interference from other active ingredients (hydrocortisone and menthol) does not occur.

Department of Chemistry, Faculty of Science. Banaras Hindu University, Varanasi-221 005 Manuscript received 3 June 1980, revised 25 November 1980, accepted 23 February 1981 2-Methoxyethanol complexes of tin(IV) and titanium(IV) have been synthesized and their probable structures on the basis of the ligand conformations have been discussed with the help of spectral data.

Three techniques--ultraviolet, high pressure liquid chromatography (HPLC) and acid dye--were compared as stability-indicating assay methods. Investigations on six drugs (codeine phosphate, ephedrine hydrochloride, morphine sulfate, procaine hydrochloride, pyrilamine maleate and thiamine hydrochloride) indicate that HPLC is the most reliable method.

Fluoro-β-diketone derivatives of titanium of the general formula (OR) 4-n Ti [OC(CF 3 ) = CHCOR'] n (R = Et and Pr 1 ; R' = CF 3 . Ph and C 4 H 3 S and n = 1 or 2), have been synthesized by the reaction of titanium alkoxides with fluoro-β-diketones. A few interchange reactions with tertiary butyl or amyl alcohols have also been studied.

The development of a simple, shorter and more accurate method than the NF method for the determination of benzyl benzoate in Benzyl Benzoate Lotion NF is discussed. Hydrolyzed benzyl benzoate was measured spectrophotometrically. Interference from other ingredients of the lotion, oleic acid and triethanolamine was almost negligible. The proposed method was completed in approximately 15 minutes, as opposed to the two hours required by the NF procedure.

N-Methylaminoalkoxides of zirconium of the type, Zr(OPri)4-n(O.CHR′.CH2.NR″R′)n, where R′ = R′ = H, R′ = Me; R′ = H, R′ = R′ = Me; R′ = R′ = R′ = Me; and n = 1–4, have been synthesized by the reactions of zirconium isopropoxide with aminoalcohols. These are characterized by elemental analyses and IR spectra. Insertion reactions of zirconium aminoalkoxides have been studied for the first time and have been shown to yield interesting derivatives with Zr-N bonds.

Chemistry Department, University of Rajasthan, Jaipur-302 004 Manuscript received 23 October 1979, accepted20 December 1979 Mono-organotin (IV) Derivatives of Hydroxamic Adds &nbsp

Department of Chemistry, Faculty of Science, Banaras Hindu University, Varanasi-221 005 Manuscript received 29 July 1981, revised 30 November 1981, accepted 7 January 1982 Metal Complexes of Sulfur-Nitrogen Chelating Agents : Organotin(IV) Derivatives of Diethylaminomethyl Ester of 2-Amino-1- cyclopentene-1-carbodlthioic Acid.

Using Wilson's GF-matrix method as modified by Higgs for infinite helical polymers, dispersion curves and the frequency distribution function have been calculated for poly-L-proline II chain. Infrared spectrum is obtained and a Urey-Bradley force field, which provides best fit with the observed frequencies, is evaluated. The result are discussed from the viewpoint of the conformational characteristics of forms I and II.

A detailed study has been made of the reaction between stannic chloride and acetylacetoie. In the re-fluxing benzene, the reaction in varying molar ratios yields a light brown crystalline solid, corresponding to SnCI2(AcAc)2 (I) which has been shown to be a simple monomeric, non-conducting compound. In cold, a product, corresponding in analysis to SnCl4.HAcAc, is obtained, to which the plausible formula [HAcAo)2 SnCl2]SnCl6 has been assigned. This has been confirmed by its observed conductance in nitrobenzene as well as by the isolation of an identical product by adding stannic chloride to [(HAcAc)2SnCl2]Cl2, obtained by passing hydrogen chloride in a solution of (I).

Chemical Laboratories, University of Rajasthan, Jaipur Received 6 September 1971 Potentiometric titrations of dialkyltin dichloride with chromotropic acid (sodium salt) in varying molar ratios have been carried out. The formation of only dialkyltin monochloromo­tropate chelates have been indicated in the lower pH range.

Halide Alkoxides of Tin(IV)

A complete normal coordinate analysis, infrared absorption, and inelastic neutron scattering studies on α-glycylglycine are reported. A Urey-Bradley force field which is also valid for N-deuterated sample is obtained. Assignments in the low-frequency region are based on inelastic neutron spectrum obtained in one phonon and cubic approximation.

Reactions of Stannic Isopropoxide with Trimethylacetoxysilane.

Reactions of Sn(OBut)4 with methanol and ethanol have revealed a greater reactivity of the former. These reactions have yielded mixed alkoxides (OBut)3 Sn(OR), (OBut)2,Sn(OR)2, and (OBut)Sn(OR)3or Et). All these mixed alkoxides undergo dispreportionation on heating under reduced pressure, the most stable ones being the tri-alkoxy-mono-t.butoxy compounds. Stannic-t-butoxide, used in these reactions, has been synthesised by a new method involving treatment of the tetra-ethoxide with t-butyl acetate.

Dispersion curves for the polyglycine I chain are calculated for both the in‐plane and out‐of‐plane modes of vibration, and the force constants are fitted by comparison with observed infrared frequencies. Frequency distributions for polyglycine I and polyglycine II are calculated from inelastic neutron scattering. The intensity difference of the C–N torsional band between polyglycine I and polyglycine II suggests the presence of additional C–H···O‐type hydrogen bonding between chains in the helical (II) form. An estimate of the sum of conformational and lattice energy difference in the two forms is made.

A number of di-isopropoxy mono-glycollate and diglycollate derivatives of tin have been described for the first time by the reaction between stannic isopropoxide and various glycols in 1:1 and 1:2 molar ratios. A few mixed ethylene glycollateshave also been isolated. With a view to synthesizing some volatile deriva­tives the reactions of monomeric stannic tertiary butoxide with some of these branched glycols were also investigated. The determination of molecular weights showed them to be polymeric.

Dispersion curves and frequency distribution for poly-L-hydroxyproline (PLHP) chain were obtained using Wilson's GF matrix method as modified by Higgs. These are compared with those of poly-L-proline II and polyglycine II, which also have three-fold screw symmetry. Ring and skeletal modes characteristic of PLHP are identified and the assignments of observed infrared and Raman frequencies are reported. Urey-Bradley force constants were evaluated.

Bis(1,3,5,2-oxadiazaborol-2-yloxy)tetrabutyldistannoxanes have been synthesized by the reaction of amidoxime, boric acid and dibutyltin oxide. A probable structure for the dimeric species has been proposed on the basis of molecular weight and IR spectral data.

Petticolas and Dowley have reported an approximate calculation of the acoustical phonon spectrum of a simplified helical model in the harmonic approximation1. The purpose of the present communication is to report that the normal modes of motion have already been obtained for a number of polymeric molecules of greater complexity than the model considered by the authors and the corresponding phonon spectra have been measured by the inelastic neutron scattering technique2. Moreover, Petticolas and Dowley's model involves only intrachain hydrogen bonded helix and is quite inapplicable to the polyglycine molecule which they discuss because in this molecule only interchain hydrogen bonds are present3. In other polypeptides, which exist in the helix form, the-presence of bulky side groups is expected to change-appreciably the dispersion of the low frequency modes, of vibration.

Alkoxides of titanium react exothermally with oximes and diethylhydroxylamine to give complexes of the formula, Ti(OR)4–x(L)x[x= 1–4; R = Pri when LH = oxime; R = Et, Pri, and But when LH = Et2NOH]. Alcoholysis of some of these give the corresponding t-butoxy-derivatives. I.r. spectra have been recorded and molecular weights determined.

Oxotrichlorobis(triphenylphosphine)rhenium(V) reacts with monobenzoylhydrazine and dibenzoylhydrazine in benzene–ethanol in the presence of hydrochloric acid to give [N-benzoylhydrazido(3-)-O,N′]dichlorobis(triphenylphosphine)rhenium(V). The chelate ring is opened by a number of nucleophiles to give rhenium(III) benzoylazo-complexes. Certain tertiary and ditertiary phosphines react further in alcoholic solvents to yield rhenium(I) dinitrogen complexes. In the presence of a ketone [ReOCl3(PPh3)2] reacts with monobenzoylhydrazine to give a chelate complex derived from the ketone hydrazone.

Alkylthio derivatives of antimony(111) Sb(SR)3 (R = Et, Pr, Pr1, Bu, Bu1, Bus, But, and Pentt) have been synthesized in high yields by reaction of SbCl3 with thiol in the presence of ammonia. An attempt has been made to throw some light on the mode of their decomposition.