摘要:

AbstractThe reaction of 3‐mercapto‐4‐arylideneamino‐1,2,4‐triazoles2b‐d,3a‐dwith ethyl bromoacetate and/or phenacyl bromide in hot DMF and triethylamine affords the stereochemically pure 7‐acyl‐6‐aryl‐6,7‐dihydro‐5H‐1,2,4‐triazolo[3,4‐b][1,3,4]thiadiazines4b‐d,5a‐d,6b,din which the consecutive hydrogen atoms N(5)H‐C(6)H‐C(7)H are cis to each other. This stereochemistry was determined by1H NMR spectroscopy and confirmed by comparison with the spectrum of 3,6‐diphenyl‐6,7‐dihydro‐5H‐1,2,4‐triazolo[3,4‐b][1,3,4]thiadiazine10. The latter was prepared by NaBH4reduction of 3,6‐diphenyl‐5H‐1,2,4‐triazolo[3,4‐b][1,3,4]thiadiazine9. The reported reactions offer two interesting s

ISSN:1042-7163    

DOI:10.1002/hc.520050402

出版商:VCH Publishers, Inc.    

年代:1994

数据来源: WILEY

摘要:

AbstractTri‐ and diphenyllead(IV) diorganophosphinodithioates, PhnPb(S2PR2)4−n(n = 2 and 3; R = Me, Et, Ph) were prepared by reacting the corresponding organolead(IV) chloride with the sodium or ammonium salt of the phosphinodithioic acid. The title compounds were investigated by infrared,1H and31P NMR, and mass spectroscopy, and possible structures were proposed. The diphenyllead(IV) phosphinodithioates, Ph2Pb(S2PR2)2, undergo decomposition on standing or on moderate heating, the least stable being the ethyl derivative. The process was monitored by using1H and31P NMR spectroscopy, and a reaction pathway leading to Ph3PbS2PR2, Pb(S2PR2)2, and R2P(S)SPh was establis

ISSN:1042-7163    

DOI:10.1002/hc.520050403

出版商:VCH Publishers, Inc.    

年代:1994

数据来源: WILEY

摘要:

AbstractThe reaction of di(isopropyl)aminophosphaethyne1with iodomethane or the methyl ester of trifluormethylsulfonic acid (methyl triflate) yields the ionic 1λ3, 3λ3‐diphosphetene derivatives+X−(2a: X = I;2b: X = CF3SO3). On the basis of NMR spectroscopic and X‐ray diffraction studies, the cation can be described as a combination of an amino‐2‐phosphaallylic cation and its methylated

ISSN:1042-7163    

DOI:10.1002/hc.520050404

出版商:VCH Publishers, Inc.    

年代:1994

数据来源: WILEY

摘要:

AbstractThe reaction mechanism of controlled hydrolysis of the inorganic ring system (NPCl2)2NSOCl in the presence of KCl and 18‐crown‐6 has been revised and is explained from steric constraints rather than from electronic considerations. The X‐ray structure of one of the hydrolysis products, [KC12H24O6]+‐[NHPO2NPCl2NSOCl]−, shows a dimeric structure of two centrosymmetrically related formula units kept together by hydrogen bridges and K … O coordination. Crystals are monoclinic, space group C2/c with a = 25.698(5), b = 8.223(2), c = 23.665(4) Å, β = 106.03(1)°, V = 4806(2) Å3, and Z = 8. The final R and Rwvalues are 0.048 and 0.04

ISSN:1042-7163    

DOI:10.1002/hc.520050405

出版商:VCH Publishers, Inc.    

年代:1994

数据来源: WILEY

摘要:

AbstractThe reactions of Cl3PNP(O)Cl2(1) with primary and secondary amines have been studied. The following monophosphazenes, (RRN)3PNP(O)(NRR)2, and bis(phosphinoyl)amines, [(RRN)2P(O)]2NH were isolated: NRR = NHCH2Ph, Net2, NH(CH2)2CH3groups for monophosphazenes, and Net2, NH(CH2)2CH3for phosphinoyl amines. The unexpected geminal phosphazene, Cl(RRN)2PNP(O)Cl2, {RRN = N[CH(CH3)2]2}, was also obtained in moderate yield. The spectral data (IR,1H,13C, and31P NMR, and MS) are presented. The structure of 1‐(dichlorophosphinyl)‐2‐chloro‐2,2‐bis(diisopropylamino)phosphazene (5) was determined by X‐ray crystallography. The basicities of these and related compounds in nonaqueous nitrobenzene solution were obtained by p

ISSN:1042-7163    

DOI:10.1002/hc.520050406

出版商:VCH Publishers, Inc.    

年代:1994

数据来源: WILEY

摘要:

AbstractA series of 2‐anilino‐2‐thio‐1,3,2‐oxazaphospholanes derived from ephedrine has been synthesized and conformationally studied by proton NMR and X‐ray crystallography. The NMR data can be interpreted in terms of twist‐envelope conformations in which the anilino substituents on phosphorus adopt predominantly equatorial positions. X‐ray crystal structures of (2R,4S,5S)‐2‐anilino‐2‐thio‐3,4‐dimethyl‐5‐phenyl‐1,3‐2‐oxazaphospholane, (2R,4S,5S)‐2‐(4‐fluoroanilino)‐2‐thio‐3,4‐dimethyl‐5‐phenyl‐1,3,2‐oxazaphospholane, and (2R,4S,5S)‐2‐(4‐methoxyanilino)‐2‐thio‐3,4‐dimethyl‐5‐phenyl‐1,3,2‐oxazaphosholane have been carried out, and these compounds adopt envelop, twist‐envelope, a

ISSN:1042-7163    

DOI:10.1002/hc.520050407

出版商:VCH Publishers, Inc.    

年代:1994

数据来源: WILEY

摘要:

AbstractUnlike the N‐sulfonylsulfimide1a, which does not react with diaryl ditellurides2even at 180°C, the selenimide1b, and tellurimides1c,dconvert quantitatively compounds2to N,N‐bis‐(N′‐p‐tosylimidoarenetellurinyl)‐p‐tosylamides4a,bin refluxing benzene. The reactivity of N‐sulfonylchalcogenimides1increases in the order S

ISSN:1042-7163    

DOI:10.1002/hc.520050408

出版商:VCH Publishers, Inc.    

年代:1994

数据来源: WILEY

摘要:

AbstractThe structure of the title compound1has been determined by X‐ray analysis. The following crystal data were found: orthorhombic, P212121, a = 5.243(2), b = 24.864(4), and c = 37.083(6) Å. Three molecules of the compound with four molecules of water are present in the independent part of the unit cell. The sugar ring puckering is3E for the molecules A and C and3T2for the molecule B. The conformation of the hydroxymethylene group is g+and g−for B and A, C, respectively. The torsion angles χ for all molecules are in the range of the anti conformation. In the crystal lattice of1both the intra‐and intermolecular hydrogen bonding system

ISSN:1042-7163    

DOI:10.1002/hc.520050409

出版商:VCH Publishers, Inc.    

年代:1994

数据来源: WILEY

摘要:

AbstractThe triazaphosphole1adds sulfur along with HCl or H2S to yield, respectively, the dihydrotriazaphosphole thiochloride4and sesquisulfide5(two diastereomers). In pyridine solution,1adds sulfur alone to yield the trimer of a triazaphosphole monosulfide7. Its central cyclotriphosphazane trisulfide ring has a trans structure and a boat conformation.

ISSN:1042-7163    

DOI:10.1002/hc.520050410

出版商:VCH Publishers, Inc.    

年代:1994

数据来源: WILEY

摘要:

AbstractThe reactions of 2‐chloromethylthiophene (an analog of a benzyl halide) with lithium trialkylalkynylborates gave, after protonation, E‐alkenes with a (2‐thenyl) substituent in good yields, and the reaction stereo‐selectivity was different from that of the reaction of benzyl bromide with an alkyny

ISSN:1042-7163    

DOI:10.1002/hc.520050411

出版商:VCH Publishers, Inc.    

年代:1994

数据来源: WILEY