共查询到10条相似文献,搜索用时 109 毫秒
1.
Dr. Michael Gock Dr. Michael Lutter Dr. Anna Pintus Dr. Dieter Schollmeier Prof. Dr. Massimiliano Arca Prof. Dr. Vito Lippolis Prof. Dr. Klaus Jurkschat 《Chemistry (Weinheim an der Bergstrasse, Germany)》2022,28(58):e202201447
The sequence of reactions of the phosphorus-containing aryllithium compound 5-t-Bu-1,3-[(P(O)(O-i-Pr)2]2C6H2Li (ArLi) with Ph2PCl, KMnO4, elemental sulfur and elemental selenium, respectively, gave the aryldiphenylphosphane chalcogenides 5-t-Bu-1,3-[(P(O)(O-i-Pr)2]2C6H2P(E)Ph2 ( 1 , E=O; 2 , E=S; 3 , E=Se). Compound 1 partially hydrolysed giving [5-t-Bu-1-{(P(O)(O-i-Pr)2}-3-{(P(O)(OH)2}C6H2]P(O)Ph2 ( 4 ). The reaction of ArLi with PhPCl2 provided the benzoxaphosphaphosphole [1(P), 3(P)-P(O)(O-i-Pr)OPPh-6-t-Bu-4-P(O)(O-i-Pr)2]C6H2P ( 5i ) as a mixture of the two diastereomers. The oxidation of 5i with elemental sulfur gave the benzoxaphosphaphosphole sulfide [1(P), 3(P)-P(O)(O-i-Pr)OP(S)Ph-6-t-Bu-4-P(O)(O-i-Pr)2]C6H2 ( 5 ) as pair of enantiomers P1(R), P3(S)/P1(S), P3(R) of the diastereomer (RS/SR)- 5 ( 5b ). The aryldiphenylphosphane 5-t-Bu-1,3-[(P(O)(O-i-Pr)2]2C6H2PPh2 ( 6 ) was obtained from the reaction of the corresponding aryldiphenylphosphane sulfide 2 with either sodium hydride, NaH, or disodium iron tetracarbonyl, Na2Fe(CO)4. The oxidation of the aryldiphenylphosphane 6 with elemental iodine and subsequent hydrolysis yielded the aryldiphenyldioxaphosphorane 9-t-Bu-2,6-(OH)-4,4-Ph2-3,5-O2-2,6-P2-4λ5-P-[5.3.1.0]-undeca-1(10),7(11),8-triene ( 7 ). Both of its diastereomers, (RR/SS)- 7 ( 7a ) and (RS/SR)- 7 ( 7b ), were separated as their chloroform and i-propanol solvates, 7a ⋅2CHCl3 and 7b ⋅i-PrOH, respectively. DFT calculations accompanied the experimental work. 相似文献
2.
K. C. Kumaraswamy Sudha Kumaraswamy Praveen Kommana N. Satish Kumar K. Senthil Kumar 《Journal of Chemical Sciences》2002,114(4):367-377
The compounds [CH2(6-t-Bu-4-Me-C6H2O)2]PCl (1), (OCH2CMe2CH2O)-PCl (2), and [ClPN(t-Bu)]2 (3) have been utilized as precursors in the synthesis of (i) new pentacoordinate phosphorus compounds [e.g. CH2(6-t-Bu-4-Me-C6H2O)2 P(NRR′)(O2C6C14), CH2(6-t-Bu-4-Me-C6H2O)2PX[OC(O-i-Pr)N=N(C(O)O-i-Pr)],(ii) cyclic phosphates and their complexes [e.g. imidazolium+CH2(6-t-Bu-4-Me-C6H2O)2PO2
-.MeOH], (iii) new cycloaddition products [e.g. CH2(6-t-Bu-4-Me-C6H2O)2PC(CO2Me)C(CO2Me)C(O)N, (iv) macrocyclic compounds [e.g. [(t-BuN)P]2[-OCH2CMe2CH2O-]h2] and (v) phosphonates [e.g. (OCH2CMe2CH2O)P (O)CH2C(CN)=CHC5H4FeC5H5]. The synthetic and structural aspects of these new products are discussed. 相似文献
3.
K. V. P. Pa Van Kumar K. Praveen Kumar M. Vijjulatha K. C. Kumara Swamy 《Journal of Chemical Sciences》2004,116(6):311-317
The compounds S(6-t-Bu-4-Me-C6H2O)2P(O)Cl (1), CH2(6-t-Bu-4-Me-C6H2O)2P(O)Cl (2) and (2,2′-C20H12O2)P(O)Cl (3) react with diazabicycloundecene (DBU) to give rise to, predominantly, the phosphonate compounds [S(6-t-Bu-4-Me-C6H6O)2P(O)(DBU)]+[Cl]− (4), [CH2(6-t-Bu-4-Me-C6H2O)2P(O) (DBU)]+[Cl]− (5) and [(2,2′-C20Hi2O2)P(0)(DBU)]+[Cl]- (6). The first two compounds could be isolated in the pure state. In analogous reactions of 1 and 2 with diazabicyclononene
(DBN) or N-methyl imidazole, only the pyrophosphates [S(6-t-Bu-4-Me-C6H2O)2P(O)]2O (7) and [CH2(6-t-Bu-4-Me-C6H2O)2P(O)]2O (8) could be isolated, although the reaction mixture showed several other compounds in the phosphorus NMR. A possible pathway
for the formation of phosphonate salts is proposed. The X-ray crystal structures of4,7 and8 are also discussed. 相似文献
4.
Markus Henn Bernard Mahieu Arnaldo Cinquantini 《Journal of organometallic chemistry》2006,691(8):1560-1572
The intramolecularly coordinated heteroleptic stannylene [4-t-Bu-2,6-{P(O)(O-i-Pr)2}2C6H2]SnCl serves as synthon for the synthesis of the ferrocenyl-bridged bis(diorganostannylene) [4-t-Bu-2,6-{P(O)(O-i-Pr)2}2C6H2SnC5H4]2Fe (1) which in turn reacts with W(CO)6 and Cr(CO)4(C7H8) to provide the corresponding transition metal complexes [4-t-Bu-2,6-{P(O)(O-i-Pr)2}2C6H2Sn{W(CO)5}C5H4]2Fe (2) and [4-t-Bu-2,6-{P(O)(O-i-Pr)2}2C6H2SnC5H4]2Fe · Cr(CO)4 (3), respectively. Reaction of compound 1 with sulphur and atmospheric moisture gave, under partial tin-carbon and oxygen-carbon bond cleavage, a tetranuclear organotin-oxothio cluster 5. All compounds were characterized by 1H, 13C, 31P, and 119Sn NMR, and IR spectroscopy, as well as by single-crystal X-ray diffraction analysis. Compounds 1 and 3 were also investigated by Mössbauer spectroscopy. Cyclovoltametric studies reveal the influence of the organostannyl moieties on the redox-behaviour of compounds 1-3 in comparison with unsubstituted ferrocene. 相似文献
5.
K.C. Kumara Swamy G. Gangadhararao R. Rama Suresh N.N. Bhuvan Kumar Manab Chakravarty 《Journal of organometallic chemistry》2010,695(7):1042-382
Phosphine-activated reactions of alkynes/alkenes/allenes as well as the Mitsunobu reaction involve a rich phosphorus chemistry. With the aid of simple cyclodiphosphazanes, characterization of many compounds analogous to the proposed intermediates in such reactions has been accomplished. Use of a cyclodiphosphazane in Pd-catalyzed N-arylation reactions is highlighted. Results on molecular non-stoichiometry in phosphorus compounds and on the use of chiral phosphorus systems are discussed. Synthesis of allenylphosphoramides involving a cyclodiphosphazane is also described. X-ray structures of the new compounds [(t-BuNH)(PhCH2CH(CN)CH2-)P(μ-N-t-Bu)2P(NH-t-Bu)]+[HCO3]− (13), [(t-BuNH)P(μ-N-t-Bu)2P(N-t-Bu)-C(CH2)CH(C6H4-4-Me)-P(O)(OCH2CMe2CH2O)] (18), [(i-PrNH)P(μ-N-t-Bu)2P(N-i-Pr)-N(CO2-i-Pr)-NH(CO2-i-Pr)] (24), [(S)-(2-OH-1-C10H6-1′-C10H6-2′-O-P(O)(NH-t-Bu)2] (36) and [(t-BuNH)(O)P(μ-N-t-Bu)2P(O)(CHCCMe2)] (40) are also reported. 相似文献
6.
L. V. Klyba N. A. Nedolya O. A. Tarasova E. R. Zhanchipova O. G. Volostnykh 《Russian Journal of Organic Chemistry》2010,46(7):1038-1048
The mass spectra of previously unknown 1-alkyl(cycloalkyl, aryl)-3-alkoxy(aryl)-2-methylsulfanyl-1H-pyrroles were studied. Fragmentation of all 3-alkoxy-substituted pyrroles under electron impact (70 eV) follow both ether
and sulfide decomposition paths; In particular, 1-R-substituted 3-methoxy-2-methylsulfanyl-1H-pyrroles (R = Me, Et, i-Pr, s-Bu, cyclo-C5H9, cyclo-C6H11, Ph) lose methyl radical group from both methoxy and methylsulfanyl groups. The mass spectra of 1-sec-butyl- and 1-cycloalkylpyrroles also contained a strong peak (10–49%) from odd-electron [M — C
n
H2n
]+· ion formed via cleavage of the N-R bond with synchronous hydrogen transfer. Cleavage of the O-Alk bond in the fragmentation
of 3-alkoxy-1-isopropyl-2-methylsulfanyl-1H-pyrroles (Alk = Et, i-Pr, t-Bu) was accompanied by rearrangement process leading to the corresponding alkene and odd-electron 1-isopropyl-2-methylsulfanyl-1H-pyrrol-3-ol ion. The main fragmentation path of 1-alkyl-2-methylsulfanyl-3-phenyl-1H-pyrroles (Alk = Me, i-Pr) under electron impact involves dissociation of the S-Me bond with formation of rearrangement 1H-[1]benzothieno[2,3-b]pyrrol-8-ium ion. 相似文献
7.
Synthesis of 1,2,3,4-tetrazine 1,3-dioxides annulated with 1,2,3-triazoles and 1,2,3-triazole 1-oxides 总被引:1,自引:0,他引:1
Alexey A. Voronin Victor P. Zelenov Aleksandr M. Churakov Yurii A. Strelenko Ivan V. Fedyanin Vladimir A. Tartakovsky 《Tetrahedron》2014
1,2,3,4-Tetrazine 1,3-dioxides annulated with 1,2,3-triazoles and 1,2,3-triazole 1-oxides have been synthesized by the reaction of 4-amino-5-(tert-butyl-NNO-azoxy)-2-R-2H-1,2,3-triazoles (R=Me, i-Pr, t-Bu) and their 1-oxides (R=H, Me, Et, i-Pr) with the HNO3/H2SO4/Ac2O system. Their thermal stability, spectroscopic, and X-ray properties have been studied. 相似文献
8.
G. I. Borodkin A. Yu. Vorob’ev M. M. Shakirov V. G. Shubin 《Russian Journal of Organic Chemistry》2011,47(6):889-896
Treatment of 2-X-substituted pyrazines [X = H, Me, Et, Pr, i-Pr, t-Bu, MeCH(OH), H2N, AcNH] with O-mesitylenesulfonylhydroxylamine gave the corresponding 2-X- and 3-X-(1-amino)pyrazin-1-ium mesitylenesulfonates. 2-Alkylpyrazines
(X = Me, Et, Pr, i-Pr) displayed a correlation between the logarithms of the concentration ratio of 2- and 3-substituted cations and substituent
steric constants. Wider series of substituted pyrazines [X = H, Me, Et, Pr, i-Pr, MeCH(OH), H2N, AcNH] conformed to a multiparameter correlation between the logarithms of the concentration ratio of 2- and 3-substituted
cations, on the one hand, and substituent constants σI, σRo, and E
so, on the other. The obtained data on the regioselectivity of amination of pyrazines were interpreted in terms of DFT/PBE/3Z
quantum-chemical calculations. 相似文献
9.
Contributions to the Chemistry of Phosphorus. 159. On the Reaction of the Diphosphaborirane (t-BuP)2BN(i-Pr)2 with Potassium or Potassium Naphthalenide The reaction of (t-BuP)2BN(i-Pr)2 with potassium or K-naphthalenide in tetrahydrofuran leads to K(t-Bu)P? ;BN(i-Pr)2? P(t-Bu)K ( 1 ) via P? ;P bond cleavage of the three-membered ring skeleton. Above ? 78°C 1 changes into the asymmetric compound K(t-Bu)P? ;P(t-Bu)? BHN(i-Pr)2 ( 2 ). In dimethoxyethane additionally the monometallated diphosphaborirane K(t-Bu)P2BN(i-Pr)2 ( 3 ) is formed. 1 and 3 , which could be isolated free from other phosphorus containing compounds, as well as the corresponding silylphosphanes Me3Si(t-Bu)P? ;BN(i-Pr)2? ;P(t-Bu)SiMe 3 ( 4 ) and Me3Si(t-Bu)P2BN(i-Pr)2 ( 5 ) were characterized by NMR spectroscopy. Protolysis of 3 or 5 leads to a decomposition of the three-membered ring skeleton with formation of H(t-Bu)P? ;PH2. 相似文献
10.
Ośmiałowski Borys Kolehmainen Erkki Kalenius Elina Behera Babita Kauppinen Reijo Sievänen Elina 《Structural chemistry》2011,22(5):1143-1151