Chlorosulfination of Aromatic Methyl Ethers with Thionyl Chloride

1985 ◽  
Vol 38 (8) ◽  
pp. 1209 ◽  
Author(s):  
KH Bell

Aromatic sulfinyl chlorides have been prepared in high yield by direct chlorosulfination of some aromatic ethers (1,3-dimethoxybenzene, 2- methyl- and 4-chloro-1,3-dimethoxybenzene, 1,2,3-trimethoxybenzene, 1- and 2-methoxynaphthalene, 1,5-, 1,7-, 2,6- and 2,7- dimethoxynaphthalene ) with thionyl chloride alone at or below room temperature. Under the same conditions, 1,4-dimethoxynaphthalene and 1,3-dimethoxy-5-methylbenzene yield chlorinated starting materials and sulfides. 1,3,5-Trimethoxybenzene yields chlorinated starting material, sulfide, and a chlorinated disulfide. Some other ethers (e.g. anisole, 1,2- and 1,4-dimethoxybenzene, 5-chloro-1,3-dimethoxybenzene) are unreactive under these conditions.

2021 ◽  
Vol 6 (1) ◽  
pp. 25
Author(s):  
Sanghamitra Ghosal ◽  
Partha Bhattacharyya

The systematic optimization of surface engineering (dimensionality) indeed plays a crucial role in achieving efficient vapor-sensing performance. Among various semiconducting metal oxides, owing to some of its unique features and advantages, ZnO has attracted researchers on a global scale due to its application in various fields, including chemical sensors. The concomitant optimization of the surface attributes (varying different dimensions) of ZnO have become a sensation for the entire research community. Moreover, the small thickness and extremely large surface of exfoliated 2D nanosheets render the gas sensing material an ideal candidate for achieving strong coupling with different gas molecules. However, temperature is a crucial factor in the field of chemical sensing. Recently, graphene-based gas sensors have attracted attention due to their variety of structures, unique sensing performances and room temperature working conditions. In this work, a highly sensitive and fast responsive low temperature (60 °C)-based ethanol sensor, based on RGO/2D ZnO nanosheets hybrid structure, is reported. After detailed characterizations, the vapor sensing potentiality of this sensor was tested for the detection of ethanol. The ethanol sensor offered the response magnitude of 89% (100 ppm concentration) with response and recovery time of 12 s/29 s, respectively. Due to excessively high number of active sites for VOC interaction, with high yield synthesis process and appreciably high carrier mobility, this has paved the way for developing future generation, miniaturized and flexible (wearable) vapor sensor devices, meeting the multidimensional requirements for traditional and upcoming (health/medical sector) applications. The underlying mechanistic framework for vapor sensing, using this hybrid junction, is explained with the Energy Band Diagram.


2021 ◽  
Author(s):  
Elif Büşra Çelebi ◽  
Ferda Hacıvelioğlu

The effect of solvent polarity on the reaction of PCl5 with (Me3Si)2NH has been investigated and it is found that nonpolar solvents promote the formation of Cl3PNSiMe3, whereas the more polar chloroform gives unusual phosphazenes at room temperature.


2016 ◽  
Vol 5 (4) ◽  
Author(s):  
Ramadan Ahmed Mekheimer ◽  
Abdullah Mohamed Asiri ◽  
Afaf Mohamed Abdel Hameed ◽  
Reham R. Awed ◽  
Kamal Usef Sadek

AbstractStarting from readily available 2-naphthol, aldehydes, aryl and alkylamines, a variety of Betti bases were efficiently synthesized utilizing a catalytic amount of cerium (IV) ammonium nitrate (CAN) at room temperature. This protocol has advantages of high yield, mild reaction conditions, no environmental pollution, diversity of reactants and simple work up procedure.


1986 ◽  
Vol 235 (3) ◽  
pp. 731-734 ◽  
Author(s):  
D H Rich ◽  
M A Brown ◽  
A J Barrett

Human cathepsin B was purified by affinity chromatography on the semicarbazone of Gly-Phe-glycinal linked to Sepharose 4B, with elution by 2,2′-dipyridyl disulphide at pH 4.0. The product obtained in high yield by the single step from crude starting material was 80-100% active cathepsin B. The possibility that this new form of affinity chromatography may be of general usefulness in the purification of cysteine proteinases is discussed.


2021 ◽  
pp. 118946
Author(s):  
Junchai Zhao ◽  
Mengwei Deng ◽  
Shuaiyao Li ◽  
Zheng Guan ◽  
Yixuan Xia ◽  
...  

Synlett ◽  
2020 ◽  
Vol 31 (14) ◽  
pp. 1423-1429
Author(s):  
Takashi Matsumoto ◽  
Yuuki Fujimoto ◽  
Chisato Furukawa ◽  
Kanae Takahashi ◽  
Miho Mochizuki ◽  
...  

The SNAr reaction of 1-fluoroxanthone derivatives with alkoxide of 1,1-dimethylallyl alcohol cleanly afforded the corresponding ethers, which have thus far been unavailable. The obtained ethers underwent the Claisen rearrangement at room temperature by treatment with silica gel in toluene. This two-step protocol provides expeditious and high-yield access to xanthones possessing isoprenyl or the related allylic side chain at the C2 position.


2018 ◽  
Vol 54 (85) ◽  
pp. 12085-12088 ◽  
Author(s):  
Eko K. Sitepu ◽  
Darryl B. Jones ◽  
Youhong Tang ◽  
Sophie C. Leterme ◽  
Kirsten Heimann ◽  
...  

A novel continuous flow turbo-thin film device (T2FD) is effective in producing biodiesel in high yield from wet microalgae at room temperature.


1971 ◽  
Vol 49 (12) ◽  
pp. 2064-2072 ◽  
Author(s):  
R. A. B. Bannard ◽  
N. C. C. Gibson ◽  
J. H. Parkkari

trans-2-Acetamidocyclohexanol (1; n = 2, R = CH3) on addition to thionyl chloride in chloroform at 0° was converted rapidly and quantitatively to D,L-2-methyl-4,5-cis-cyclohexanoöxazoline hydrochloride (2; n = 2, R = CH3) judging from shifts in the methyl proton resonances of the n.m.r. spectra of the amide and the reaction solution. The intermediate chlorosulfinate was estimated to have a half-life of less than 2.25 min. The oxazoline salt was isolated in 98% yield by sublimation of the crude product in vacuo and was identified by its i.r. and n.m.r. spectra and by its facile and almost quantitative hydrolysis to cis-2-aminocyclohexanol hydrochloride. The oxazoline salts 2 (n = 1, R = CH3, [Formula: see text] and n = 2, R = C6H5, [Formula: see text]) were readily obtained in 95 % yield or better by the same general method and it was shown that the trans-2-acetamidocyclanols are the preferred starting materials for conversion to cis-2-aminocyclanol derivatives by the thionyl chloride inversion reaction. The oxazoline bases 4 (n = 1, R = CH3, [Formula: see text] and n = 2, R = CH3, [Formula: see text]) were readily obtained in high yield from the corresponding salts and differences in the i.r. and n.m.r. spectral characteristics of the salts and bases are reported.


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