Derivatives of cis-NPCl2(NSOCl)2 and (NPCl2)2NSOCl, Part X [1] Aminolysis of cis-NPCl2(NSOF)2 and (NPCl2)2NSOF

1978 ◽  
Vol 33 (9) ◽  
pp. 964-967 ◽  
Author(s):  
H. H. Baalmann ◽  
J. C. van de Grampel

The aminolysis of the ring systems cis-NPCl2(NSOF)2 and (NPCl2) 2NSOF by cyclic amines in acetonitrile at room temperature shows the S-F bond to be stable towards a nucleophilic attack. The amino derivatives are characterized by their spectral data. Structure assignments are based on 31P NMR spectroscopy.

1992 ◽  
Vol 28 (2) ◽  
pp. 173-177 ◽  
Author(s):  
I. V. Fedyunina ◽  
V. V. Plemenkov ◽  
G. Sh. Bikbulatova ◽  
L. E. Nikitina ◽  
I. A. Litvinov ◽  
...  

1995 ◽  
Vol 50 (10) ◽  
pp. 1476-1484 ◽  
Author(s):  
P. Müller ◽  
S. Huck ◽  
H. Köppel ◽  
H. Pritzkow ◽  
W. Siebert

A series of alkyl and amino derivatives of the tricyclic organoborane system 9,10-dihydro- 9.10-diboraanthracene was synthesized and examined. The reactions of 9,10-dichlor-9,10-dihydro- 9,10-diboraanthracene ( la ) with suitable reagents yield the corresponding alkyl, aryl or amino derivatives 1c-h , respectively. The compounds have been characterized by 1H, 13C and 11B NMR spectroscopy. X-ray structure analyses have shown that the amino derivatives have bent structures, while the H2N compound 1h is planar. Calculations were carried out to study the reasons for the deformation of some of the amino-substituted derivatives. These calculations indicate that steric reasons are responsible for the deformation. Electrochemical investigations show reversible reductions of the dimethyl derivative 1c leading to the radical anion and the dianion. Both anions have been structurally characterized by X-ray diffraction studies.


2017 ◽  
Vol 95 (7) ◽  
pp. 785-791
Author(s):  
Mohammad M. Mojtahedi ◽  
Kiana Darvishi ◽  
M. Saeed Abaee ◽  
Mohammad R. Halvagar

The first general procedure is described for the synthesis of novel bisarylmethylidenes of 2-methoxy-2-methyl-1,3-dioxan-5-one 1. Thus, several derivatives of 3 are obtained rapidly in high yields by reacting 1 with different aldehydes in the presence of catalytic quantities of pyrrolidine in EtOH at room temperature. Upon completion of the reactions, products are obtained directly by spontaneous precipitation avoiding time consuming and expensive chromatographic separations. All products were characterized by proton and carbon NMR spectroscopy methods, and in one case, the proposed structure was elucidated by X-ray crystallography, confirming the Z stereochemistry for the olefinic C=C bonds. Due to showing different colours in solid and solution states, products were studied for their photophysical properties as well.


1994 ◽  
Vol 49 (5) ◽  
pp. 717-720 ◽  
Author(s):  
İzzet A. Mour ◽  
Saim Özkar

Pentacarbonyl(η2-tetracyanoethylene) metal(0) complexes of chromium, molybdenum and tung­sten have been synthesized by the photochemical reaction of hexacarbonyl metal(o) with tetra- cyanoethylene in toluene at room temperature. The complexes were purified by chromatography and recrystallization, and characterized by UV- visible, IR and 13C NMR spectroscopy. Tetra- cyanoethylene is symmetrically bonded to the M(CO)5 unit through its carbon-carbon double bond as an η2-ligand. The spectral data are dis­cussed in terms of the metal → ligand π inter­action.


2005 ◽  
Vol 83 (9) ◽  
pp. 1347-1351 ◽  
Author(s):  
Leah E Breen ◽  
Norman P Schepp ◽  
C-H Edmund Tan

Irradiation of substituted 5-alkyl-4,5-epoxyvalerophenones leads to the formation of alkyl allene oxides that, in some cases, are sufficiently long-lived to be detected at room temperature by 1H NMR spectroscopy. Absolute lifetime measurements show that the size of the alkyl group has a significant influence on the reactivity of the allene oxide, with tert-butyl allene oxide having a lifetime of 24 h in CD3CN at room temperature that is considerably longer than the 1.5 h lifetime of the ethyl allene oxide. The allene oxides react rapidly with water to give α-hydroxyketones. The mechanism involves nucleophilic attack to the epoxide carbon to give an enol, which can also be detected as an intermediate by 1H NMR spectroscopy.Key words: allene oxides, mechanisms, absolute reactivity, kinetics, photochemistry.


2020 ◽  
Vol 07 ◽  
Author(s):  
Dhanaji V. Jawale ◽  
Devendra Wagare ◽  
Dinesh L. Lingampalle ◽  
Prashant D. Netankar

Background: 1,4-benzothiazine carboxylates show wide application in the field of medicinal chemistry. Therefore, we have designed convenient and efficient method for the synthesis of 1,4-benzothiazine carboxylates. Objective: Synthesis of 1,4-benzothiazine carboxylates and its guanidines by simple and facile method using efficient catalyst. Method: Derivatives of 1,4-benzothiazine carboxylates were synthesized by cyclocondensing β-keto esters with 2- aminobenzenethiols using CAN as a catalyst at room temperature. 1,4-benzothiazine caboxylate,condensed with guanidine hydrochloride in the presence of sodium methoxide in DMF to obtained new 3-substituted-l-4Hbenzo[b][1,4]thiazine-2-carboxyguanidines (88-91%). Results: All the products were obtained with good to excellent yields within 40 min. Here, CAN oxidizes aminothiophenol into disulfide and then nucleophilic attack of enolic form of β-ketoesters on the disulphide and 1, 4-benzothiazine acetates, were obtained with good yields. Conclusion: We have designed convenient and efficient method for the synthesis of 1,4-benzothiazine carboxylates. Most remarkable features of this cyclocondensation such as use of efficient catalyst and non-volatile solvent under mild reaction condition to obtained excellent yield.


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