Sitting Out the Halogen Dance. Room-Temperature Formation of 2,2′-Dilithio-1,1′-dibromoferrocene. TMEDA and Related Lithium Complexes: A Synthetic Route to Multiply Substituted Ferrocenes

Author(s):  
Ian R. Butler
Author(s):  
Thomas E. Shaw ◽  
Alfred P. Sattelberger ◽  
Titel Jurca

The true identity of the diethyl ether adduct of tungsten(IV) chloride, WCl4(Et2O) x , has been in doubt since 1985. Initially postulated as the bis-adduct, WCl4(Et2O)2, questions arose when elemental analyses were more in line with a mono-ether adduct, viz. WCl4(Et2O). It was proposed that this was due to the thermal instability of the bis-adduct. Here, we report the room-temperature X-ray crystal structure and Hirshfeld surface characteristics of trans-tetrachloridobis(diethyl ether)tungsten(IV), trans-WCl4(Et2O)2 or trans-[WCl4(C4H10O)2]. The compound crystallizes, with half of the molecule in the asymmetric unit, in the centrosymmetric space group P21/n. The W—O distance is 2.070 (2) Å, while the W—Cl distances are 2.3586 (10) and 2.3554 (10) Å.


RSC Advances ◽  
2017 ◽  
Vol 7 (6) ◽  
pp. 3161-3169 ◽  
Author(s):  
Fuhai Li ◽  
Hanqin Weng ◽  
Yun Shang ◽  
Zuoming Ding ◽  
Zheng Yang ◽  
...  

A facile, fact and green synthetic route was developed to prepare Rh nanoparticles at room temperature.


1988 ◽  
Vol 121 ◽  
Author(s):  
Atsushi Ochi ◽  
H. KENT BOWEN ◽  
Wendell E. Rhine

ABSTRACTThe reaction between ammonia and aluminum hydride (AIH3) was investigated as a possible synthetic route to aluminum nitride (AIN), using tetrahydromran (THF) as the solvent. When an excess of ammonia was employed, a white powder was obtained which was converted to AIN by calcination. However, when a stoichiometric amount of ammonia was used, a soluble intermediate was obtained. This intermediate polymerized slowly at room temperature via a condensation reaction involving the elimination of hydrogen to give a gel that could be converted to AIN.


2011 ◽  
Vol 11 (3) ◽  
pp. 2533-2536 ◽  
Author(s):  
Rui Song ◽  
Hongming Yuan ◽  
Yan Chen ◽  
Shouhua Feng

2016 ◽  
Vol 4 (30) ◽  
pp. 7332-7338 ◽  
Author(s):  
Dianpeng Cui ◽  
Qianchuan Xiang ◽  
Zhen Song ◽  
Zhiguo Xia ◽  
Quanlin Liu

We have provided and optimized a synthetic route to SrLiAl3N4phosphor. BaF2flux plays a critical role to improve room temperature and temperature-dependent spectra due to the enhancement of crystallinity.


1989 ◽  
Vol 7 (12) ◽  
pp. 411-414 ◽  
Author(s):  
Michael Schwartz ◽  
Michael Rappaport ◽  
Gary Hodes ◽  
Shimon Reich ◽  
David Cahen

2011 ◽  
Vol 04 (04) ◽  
pp. 377-381 ◽  
Author(s):  
C. D. GU ◽  
Y. J. MAI ◽  
J. P. ZHOU ◽  
J. P. TU

A new synthetic route to ~4 nm grain-sized SnO 2 was proposed which involved a homogeneous precipitation in a deep eutectic solvent (DES) at room temperature. The white SnO 2 precipitate was obtained from SnCl 2 ⋅ 2 H 2 O dissolved DES by injecting slow drop-wise H 4 N 2 ⋅ H 2 O under stirring. The as-prepared nanocrystalline SnO 2 has a Brunauer–Emmett–Teller surface area of 65.12m2/g with an average Barretl–Joyner–Halenda pore diameter of 3.5 nm. As anode for lithium ion batteries, the nanocrystalline SnO 2 electrode delivered an initial charge capacity as high as 1045 mAh/g and its capacity retention is 58% after 30 cycles.


2015 ◽  
Vol 44 (10) ◽  
pp. 4759-4764
Author(s):  
Li Yong ◽  
Min-Liang Yao ◽  
David W. Blevins ◽  
George W. Kabalka

A general synthetic route to water-soluble PEG-supported organotrifluoroborates has been developed. In the presence of air and catalytic amounts of Pd(OAc)2, the PEG-supported organotrifluoroborates undergo homo-coupling reactions smoothly at room temperature.


2001 ◽  
Vol 73 (9) ◽  
pp. 1401-1409 ◽  
Author(s):  
István Hermecz ◽  
Andrea Sánta-Csutor ◽  
Csaba Gönczi ◽  
Gergely Héja ◽  
Éva Csikós ◽  
...  

A facile convergent total synthesis of the selective, potent, and orally active V2 non-peptide antagonist, SR-121463, was developed by modification of the discovery route. One of the late intermediates, the sulfonyl chloride 1, was synthesized from 3-hydroxybenzoic acid (19) by regioselective sulfonation, O-methylation and amidation in four steps. Another late intermediate, indolin-2-one 2, was prepared from p-phenetidine (8) through the indolin-2-one 16, where the cyclohexanone moiety of 27 was introduced into the active 3-methylene group of 16 by sequential transformation using methyl acrylate and KOtBu. After formation of the cyclic ketal moiety of 13, its ring-opening was achieved by using NaBH4 in the presence of CCl3COOH. The morpholino group in 2 was introduced in accordance with the discovery approach, starting from the 2-hydroxyethoxy derivative 14 through the tosyloxy derivative 15 with morpholine in a one-pot reaction. In this way, the indolin-2-one 2 was synthesized from 8 in six steps. Finally, acylation of the indolin-2-one 2 was achieved with the sulfonyl chloride 1 in the presence of KOtBu in dimethyl sulfoxide (DMSO) at room temperature. This synthetic route proved to be applicable for the large-scale synthesis of SR-121463.


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