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1.
On the Reaction of Perfluoro Isobutene with Thiazylfluoride and Thiazyltrifluoride From thiazylfluoride (1) and perfluoro-isobutene (2) (CF3)3C? N?S?N? S? C(CF3)3 (4) isr formed in the presence of CsF. With NSF3NSF2C(CF3)3 (8) is obtained, which isomerizes above 100°C to (CF3)3CNSF2 (9). In contrast to 9, with fluoro Lewis-acids 8 forms 1:1 adducts (CF3)3CSF2N · MF5 (M = As, Sb (10a), (10b)). In 50% aqueous KOH 9 hydrolyses to give the amine (CF3)3CNH2.  相似文献   

2.
Reactions of NN-Dihaloperfluoroalkaneamines with Sulfur and Sulfur Derivatives Reactions of NN-Dihaloperfluoroalkaneamines RfNX2 (Rf = CF3, C2F5; X = Cl, Br) with S8, S4N4 and A = SX2 (A = RfN, O) are described. The products isolated are: Sulfurdihalideimides RfNSX2 (Rf = CF3, C2F5; X = Cl, Br), Sulfurdiimides RfNSNRf and Bis(sulfurdiimido)sulfides (RfNSN)2S(Rf = CF3, C2F5). Thionylimides RfNSO were not obtained in preparative quantities.  相似文献   

3.
Reaction of Adipic Acid Diamide with Phosphorus Pentachloride The reaction of adipamide (I) with phosphorus pentachloride in a solvent leads to (Cl3P?NCCl2CCl2CH2)2 (II). The stages of the reaction are: 1. chlorination of the keto and methylen groups 2. formation of the ? N?PCl3 group. This result is a supplement of the existing conception about the course of the reaction of carboxylic acid amides with phosphorus pentachloride. The reaction of (I) with PCl5 without any solvent has been reproduced and the course of reaction has also been investigated. This reaction gives mainly NC(CH2)4CN. The resulting product of a careful hydrolysis of (II) is (Cl2OPN?CClCl2CH2)2. A total hydrolysis gives back (I).  相似文献   

4.
On the Reaction of Phosphorus(III) Fluorides with Phenyl Azide The reaction of phenyl azide with phosphorus(III) fluorine compounds was found to proceed according to the principle of a Staudinger reaction producing, normally, fluorine-containing N-phenylphosphine imides. From diethylamino difluorophosphine and phenyldifluorophosphine the dimers, [(Et2N)F2PNPh]2 and [PhF2PNPh]2, were obtained with phenyl azide. These compounds have previously been prepared by a different route. The compounds were characterized by elemental analysis, determination of the molecular weight, either cryoscopically or by mass spectrometry as well as through their n.m.r. spectra (1H, 19F and 31P).  相似文献   

5.
The Reaction of Cyclophosphanes with Carbon Tetrachloride and Amines The cleavage of phenylcyclophosphanes with carbon tetrachloride leads to the chloro-trichloromethyl-phosphine 2a ; tetracyclohexycyclotetraphosphine decomposes in the same manner to the diphosphane 3 . Methyl-and ethylcyclophosphanes give with carbon tetrachloride the monoquaternary salts 4c and 4d . The cleavage products 5 , 2d and 6 are also formed. The tris-(amino)-phosphonium salts 7a – j and the chloromethylphosphonium chloride 8a are obtained by reaction of amines with cyclophosphanes and carbon tetrachloride. All phosphonium chlorides are isolated and charakterized as perchlorates.  相似文献   

6.
On Reactions of Alkali Hexafluorosilicates with Aluminum Oxides The reaction of Na- and K-hexafluorosilicates and α- or γ-Al2O3 has been investigated. Final reaction products are fluoroaluminates and alumosilicates. The reaction mechanism has been discussed. Influence of reaction parameters like time, temperature, layer thickness, and the effect of admixtures (fluorides, SiO2) have been regarded. Tablet-reactions show the introduction of reaction by Si? F species.  相似文献   

7.
8.
On the Formation of Polysulphane Diphosphonates by the Reaction of Monothiophosphonate with Disulphane Diphosphonate In acid solution SPO reacts with S2P2O forming higher polysulphane diphosphonates. The formation of S3P2O and S4P2O is proved by evaluation of the double labelling with 35S? 32P after high paper electrophoresis.  相似文献   

9.
Addition of amines to dibenzylidene sulfamide1 a yields the correspondingSchiff bases3 a, b and monobenzylidene sulfamide2. Reaction of several dibenzylidene sulfamides1 with various lithium-amides gives N1-substituted N2-benzylsulfamoyl-benzamidines7 a-k via an intramolecular hydride transfer reaction, whereas by treatment of1 a with sodium amide 2-benzyl-3,5-diphenyl-3,4-dihydro-2H-1,2,4,6-thiatriazine-1,1-dioxide8 is obtained, which on hydrolysis yields9 and11. Alkylation products are described, the isomeric products12a/13a and12b/13b are isolated, their structures are confirmed by synthesis, IR and NMR-spectra.
  相似文献   

10.
On the Reaction of Thiophosphoryl Chloride with Hexamethyl Disilazane On the basis of a 31P n.m.r. spectroscopic study of the reaction of PSCl3 with hexamethyl disilazane a method for the preparation of Me3SiNHP(S)Cl2( 1 ) and the diazadiphosphetidine 2 , [Me3SiNHP(S)?NSiMe3]2 has been developed. These new crystalline compounds have been characterized by i.r., Raman, 31P n.m.r. and mass spectroscopy, and their thermal behaviour has been studied. The formation and constitution of 2 are discussed, and its 1H and 29Si n.m.r. spectra are reported.  相似文献   

11.
The Reaction of Phenols with N-substituted Maleinimides Phenoxysuccinimides are formed by the base catalysed addition of phenols to N-substituted maleinimides. In the presence of catalytic amounts of tertiary aliphatic amines yields as high as 90% are obtained. A series of adducts of mono-and di-phenols to mono- and bismaleinimides is described. Pure phenoxysuccinimides are stable compounds but the basic catalysts of their formation give rise to their decomposition into the phenolic component and oligomeric maleinimide. A nucleophilic reaction mechanism both for the formation and the decomposition is discussed. A new crosslinked addition polymer from a diphenol and a bismaleinimide with a surprisingly high heat stability is described.  相似文献   

12.
13.
14.
In contrast to butyllithium, ethylmagnesium-bromide reacts with 1-phenyl-pyrazole exclusively by deprotonation, at the ortho position of the phenyl-ring. With nitriles the intermediate 2-(1-pyrazolyl)-phenylmagnesiumbromide gave good to excellent yields of 1-(2-aroyl or 2-hetaroyl-phenyl)-pyrazoles (Table 1, compounds 5a – 5i ); with ketones the corresponding methanol derivatives (Table 2, compounds 6a – 6c ) were found, whilst CO2 yielded the corresponding 1-(2-carboxyphenyl)-pyrazole ( 3 ). Surprisingly enough, 1-(o-bromo-phenyl)-pyrazole and magnesium did not yield a single product, but a mixture of 3 compounds, which on reaction with 4-benzoylpyridine gave the three alcohols 19 , 20 and 21 .  相似文献   

15.
In accordance with spectrophotometric measurements, manganese(III) acetate dihydrate reacts with dilute solutions of acetyl chloride in acetic acid through a 1:1 complex to a red-violet 1:4 compound which is unstable due to the oxidation potential of MnIII ions. The action of potassium acetate on solutions of MnIII in acetic acid in presence of a large excess of acetyl chloride leads to a dismutation of managanese(III) and initial precipitation of potassium chloromanganate(IV), K2MnCl6. During the reaction of potassium acetate with solutions of manganese(II)/acetic acid/acetyl chloride, under particular conditions, first nonsolvated potassium trichloromanganate(II), KMnCl3, is formed, which transforms during further addition of potassium ions to tetrapotassium hexachloromanganate(II), K4MnCl6.  相似文献   

16.
On Chalcogenolates. 113. Reactions of Chloramine with Carbon Disulfide and with Methylesters of Dithiocarbamic Acids The reactions of chloramine with CS2 and with H2N? CS? SCH3, CH3? NH? CS? SCH3, and (CH3)2N? CS? SCH3 have been studied. The reaction with the methylester of dithiocarbamic acid gives the known dimethyl perthiocyanate and the reaction with the methylester of N-methyldithiocarbamic acid leads to CH3S? CS? N(CH3)? C(?NCH3)? SCH3. The latter compound has been characterized by means of electron absorption spectra, infrared spectra, nuclear magnetic resonance spectra (1H and 13C), and mass spectra.  相似文献   

17.
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19.
Zusammenfassung Eine Anzahl aliphatischer und arylaliphatischer -Oximinoester deranti-Reihe wird mit Phenylisocyanat in guter Ausbeute zu den entsprechenden Urethanen umgesetzt. Im Gegensatz dazu reagieren unter den gleichen Bedingungen die Vertreter dersyn-Reihe nicht, was durch deren starke innermolekulare Wasserstoffbrücke zu erklären ist.
Some aliphatic and araliphaticanti-oximinoesters with phenyl-isocyanate give the corresponding urethanes in high yields. In contrast compounds of thesyn-series do not react under the same conditions due to their strong intramolecular hydrogen bond.


Mit 1 Abbildung  相似文献   

20.
On the Reaction of Nb3Cl8 with HCl The greenish-blue gas phase which is formed at 500–600°C by reaction of Nb3Cl8 with HCl, is caused by an equilibrium reaction, in which small amounts of NbCl5 and larger amounts of NbCl4 are formed. This is shown by photometric measurements and by thermodynamic calculations.  相似文献   

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