Triethoxy chloride

To a mixture of 0.20 mol of 1,1,4-triethoxy-2-butyne [see Chapter III, Exp. 40), 60 ml of dry THF and 50 ml of dry diethyl ether was added at -45 to -50°C a solution of 0.42 mol of ethyllithium in about 280 ml of diethyl ether (see Chapter II, Exp. 1). Stirring at -5o°C was continued for 30 min, then the reaction mixture was poured into 300 ml of saturated ammonium chloride solution. After shaking, the layers were separated and the aqueous layer was extracted twice with small portions of diethyl ether. The combined ethereal solutions were dried over magnesium sulfate and concentrated in a water-pump vacuum and the residue wasdistilled at about... 

It is clear that the ionizing power of the solvent used is important in many of these reductions. When 2,4,6-trimethylbenzyl chloride is heated with diphenylsi-lane in nitrobenzene at temperatures as high as 130°, no isodurene is formed.193 Not unexpectedly, the same lack of reactivity is reported for a series of benzyl fluorides, chlorides, and bromides substituted in the para position with nitro or methyl groups or hydrogen when they are heated in nitrobenzene solutions with triethylsilane, triethoxy silane, or diphenylsilane.193... 

A solution of 4.5 g 3,4,5-triethoxybenzyl chloride in 10 mL DMF was treated with 5.0 g sodium cyanide and heated for 1 h on the steam bath. The mixture was then poured into 100 mL H20 and the oily phase that resulted immediately crystallized. This was filtered off, washed well with H20, air dried, and distilled at 128-140 °C at 0.25 mm/Hg to yield 3.7 g of 3,4,5-triethoxy phenylacetonitri le which melted at 54-56.5 °C. There was a sharp nitrile band at 2249 cm1. Anal. (C 4H 19NO,) C,H. 

Sodium borohydride-Palladium chloride. Sodium borohydride-Rhodium(lII) chloride. Sodium borohydride-Tin(II) chloride. Sodium cyanoborohydride. Sodium 9-cyano-9-hydrido-9-borabicyclo[3.3.1]nonane. Sodium dithionite. Sodium hydride-Sodium t-amyl oxide-Zinc chloride. Sodium trimethoxyborohydride. Tetra-/i-butylammonium borohydride. Tetra-n-butylammonium cyanoborohydride. Tetra-n-butylammonium octahydrotriborate. Tri-n-butyltin hydride. Triethoxy silane. Triisobutylaluminum-Bis(N-methyl-salicyclaldimine)nickel. Zinc borohydride. REDUCTIVE CYCLIZATION Cobaloximc(I). 

Ethyl triethoxy silicon, C2H5Si(OC2H is isolated in the above manner from tetraethoxysilieon. Another method of preparation is from triethoxysilicon chloride, using sodium and zinc ethyl. The reaction mixture gives a colourless liquid with a camphor-like odour, B.pt. 158-5° 0., density at 0°C. 0 9207 it is insoluble in water, but miscible with alcohol and ether. It is not completely decomposed by alcoholic potassium hydroxide or ammonium hydroxide, but is broken up by concentrated sulphuric acid. ... 

Ethylsiliconic acid or Silico-propionic acid is obtained from ethyl triethoxy silicon using benzoyl chloride at 300 C. ... 

CMCs of these polyfluorinated surfactants are of the order of 10 5 m.47 Plots of the observed H chemical shifts versus surfactant concentration of cetyl trimethyl ammonium chloride, cetyl pyridinium chloride, cetyl dimethyl phenyl ammonium chloride, cetyl dimethyl benzyl ammonium chloride, cetyl dimethy 1-2-phenyl ethyl ammonium chloride, and cetyl dimethyl-3-phenyl propyl ammonium chloride, are sigmoidal and were fitted to a model based on the mass action. The H chemical shift-based CMC values are in excellent agreement with those determined by the surface tension method.48 The micellization processes of dodecyl trimethyl ammonium halides (chloride and bromide) studied by calorimetric titration show different behaviors at 298 K. However, these disappear at 313 K, while the results measured by the chemical shift versus surfactant concentration do not show this difference.49 The CMC of 3-aminopropyl triethoxy silane in toluene is ca. 0.47m, measured by H and l3C chemical shifts.50 The CMC of optically active potassium A -n-dodecanoyl alaminate measured by H and l3C chemical shifts is lower (11-15 him) in D20 than that in a mixed solvent of 1,4-dioxane and D20 (19mM).-51 The H chemical shift shows that the CMC of resorcinol-type calix[4] phosphoric esters having four alkyl side-chains, [4]Ar 5P-R-n, is insensitive to the length of the side-chains, n.52 The CMC values of a family of surfactants, the sodium cyclohexyl alkanoates, with different lengths of the alkanoate side-chains, were obtained from 13C chemical-shift measurements. The results show that these amphiphiles have high CMCs (0.12-1.02 m).-53... 

Im Unterschied zum Bis-[2-methyl-propyl]-aluminiumhydrid fiihrt die Reduktion mit Na-trium-hydro-triethoxy-aluminat nur bei aromatischen und heteroaromatischen Nitrilen zum Erfolg318-320. Bei aliphatischen Nitrilen lauft die Reduktion oft bis zu den Aminen weiter. Sterische Faktoren - wie sie bei der Reduktion von Nitrilen mit Zinn(II)-chlorid nach Stephen (s.S.485) oft auftreten - haben keinen EinfluB. 

For the preparation of such a modified silica gel, the complex N-3-(3-triethoxy-silylpropyl)-4,5-dihydroimidazole 1 is reacted with 1-chlorobutane to give the complex Tbutyl-3-(3-triethoxysilylpropyl)-4,5-dihydroimidazolium chloride 2. 

Important objectives of the later prodnction methods were to control the size and shape of the catalyst particles during precipitation of the magnesium chloride and to improve stabihty. Catalysts with better-controlled size and shape were based on the reaction of a precipitated magnesium chloride with titanium tetrachloride in a high-boiling-point hydrocarbon diluent at 80°C, with di-isobutyl phthalate added as an internal electron donor. " After separation, the sohd formed was reacted with more titaninm tetrachloride at 120°C, before being washed and dried. The catalyst contained between 2-3% titanium and the phthalates used were hmited to C4-C8 esters to avoid potential problems with colloid formation. The catalysts prodnced with phthalates as the internal donor had mnch higher snrface area and pore volume than when ethyl berrzoate was nsed. This method provided more active arrd stereospecifrc catalysts when used with the same triethyl aluminum co-calalyst and an external electron donor such as phenyl triethoxy silane. 

Second, l-methyl-3-[(triethoxysilyl)propyl]imidazolium chloride (TMICl) was synthesized as follows in a typical synthetic procedure a mixture of 1-methylimid-azole and 3-triethoxy-silylpropyl chloride (equalmolaramount) was heated at 80°C for 24 h under nitrogen atmosphere to synthesize TMICl. After cooling down, the pale-yellow viscous liquid was washed with ether for three times and dried under vacuum at 80°C for 24 h. 

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