Magnesium chloride-Sodium iodide

Grignard reagents-Vanadium(III) chloride, 219 Magnesium, 170, 235 Magnesium bromide, 259 Magnesium chloride-Sodium iodide,... 

A good number of alternative methods are also available in literature for the synthesis of 1,5-benzodiazepine derivatives involving the use of a variety of catalysts such magnesium oxide/ phosphorus oxychloride (MOPO) [1], ionic liquid (1,3-di-n-butylimidazolium bromide) [2], silica gel-supported cerium(lll) chloride/sodium iodide [3], Sc(OTf)3 [4], InCls [5], InBr3 [6], ceric ammonium nitrate (CAN) [7], 2,4,6-trichloro-l,3,5-triazine (TCT) [8,9], GaCl3 [10], and Zr0C2-8H20 [11] in the presence or absence of solvent(s) at room temperature. 

A mixture consisting of 0.69 g (10.5 mmoles) of zinc-copper couple, 12 ml of dry ether, and a small crystal of iodine, is stirred with a magnetic stirrer and 2.34 g (0.7 ml, 8.75 mmoles) of methylene iodide is added. The mixture is warmed with an infrared lamp to initiate the reaction which is allowed to proceed for 30 min in a water bath at 35°. A solution of 0.97 g (2.5 mmoles) of cholest-4-en-3/ -ol in 7 ml of dry ether is added over a period of 20 min, and the mixture is stirred for an additional hr at 40°. The reaction mixture is cooled with an ice bath and diluted with a saturated solution of magnesium chloride. The supernatant is decanted from the precipitate, and the precipitate is washed twice with ether. The combined ether extracts are washed with saturated sodium chloride solution and dried over anhydrous sodium sulfate. The solvent is removed under reduced pressure and the residue is chromatographed immediately on 50 g of alumina (activity III). Elution with benzene gives 0.62 g (62%) of crystalline 4/5,5/5-methylene-5 -cholestan-3/5-ol. Recrystallization from acetone gives material of mp 94-95° Hd -10°. 

Using the periodic table if necessary, write formulas for the following compounds (a) hydrogen bromide, (b) magnesium chloride, (c) barium sulfide, (d) aluminum fluoride, (e) beryllium bromide, (/) barium selenide, and (g) sodium iodide. 

To a stirred suspension of N-(2,6-dimethyl-4-oxopyridin-l-yl)pyridin-ium tetrafluoborate (0.58 g, 2 mmol) in dry acetonitrile (20 ml) under nitrogen was added trimethyl phosphite (0.25 g, 2 mmol), followed by finely divided sodium iodide (0.30 g, 2 mmol). After 1 h at 25°C, the solvent was removed under reduced pressure, and water (20 ml) was added. The mixture was extracted with methylene chloride (3 x 15 ml), and the extracts were dried over magnesium sulfate, filtered, and evaporated under reduced pressure. The residue was dissolved in ethyl acetate (40 ml), heated at reflux for 4 h, evaporated under reduced pressure, and eluted on an alumina column (grade 1, neutral) with chloroform to yield pure dimethyl pyridin-4-ylphosphonate (0.36 g, 96%) of melting point (mp) 139 to 140°C. 

Vinvlbenzvl Iodide—Vinylbenzyl chloride (20 g 0.131 mol) was added dropwise to dry sodium iodide (29.5 g 0.198 mol) in 130 mL dry acetone. The mixture was stirred at 50°C for 40 min, cooled to room temperature, and filtered. The acetone was removed by rotary evaporation, and 100 mL water and 150 mL ether were added to the solid residue. The aqueous layer was washed with ether. The combined ether layers were washed with water containing 2% sodium thiosulfate and dried over magnesium sulfate. The ether was removed by rotary evaporation and the yellow residue was dissolved in 50 mL hexane and cooled to -20°C. Within 1.5 hr, yellow crystals formed. Fast filtering with chilled glassware provided 17.1 g (53.5% of theory) of vinylbenzyl iodide. 

Major constituents (greater than 5 mg/L) Minor constituents (O.Ol-lO.Omg/L) Selected trace constituents (less than 0.1 mg/L) Bicarbonate, calcium, carbonic acid, chloride, magnesium, silicon, sodium, sulfate Boron, carbonate, fluoride, iron, nitrate, potassium, strontium Aluminum, arsenic, barium, bromide, cadmium, chromium, cobalt, copper, gold, iodide, lead, Uthium, manganese, molybdenum, nickel, phosphate, radium, selenium, silver, tin, titanium, uranium, vanadium, zinc, zirconium... 

Malmsten. l,2-Bis(2-ch1oroethoxy)ethane (21.3 g, 0.114 mol) and sodium iodide (37.0 g, 0.247 mol) in acetone (55 ml) were heated at reflux while stirring magnetically during three days. The reaction mixture was allowed to cool, it was filtered, and the filtrate was evaporated under reduced pressure. The residue was dissolved in methylene chloride (200 ml), washed with aqueous 10% sodium thiosulfate solution (2 x 100 ml), dried over magnesium sulfate, and evaporated under reduced pressure. The residual... 

Vanadium metal is prepared from pentoxide, V2O5, by reduction with calcium at elevated temperatures. Presence of iodine lowers calcium reduction temperature to 425°C because of heat of formation of calcium iodide. Pentoxide also may be converted to the trichloride, VCI3, and the trichloride reduced with magnesium metal or magnesium-sodium mixture at high temperatures to form high purity ductile metal. Alternatively, a fused mixture of vanadium chloride, sodium chloride, and hthium chloride may be electrolyzed to produce the metal in high purity. 

Glacial acetic acid. Aluminum foil. Toluene, Methylene iodide. Acetonitrile, Tetrahydrofuran, Sodium hydroxide. Acetone, Magnesium sulfate. Aluminum chloride. Chloroform Ethylenediamine, Glyoxal, Sodium nitrite. Hydrochloric acid. Nitric acid. Ethanol 4,4,4-Trinitrobutryaldehyde, Methanol, Sodium borohydride. Hydrochloric acid. Methylene chloride. Sodium bicarbonate. Magnesium sulfate... 

Formerly all the iodine was made from the ash of seaweed, and potash was a remunerative appendix to the iodine industry but just as the Stassfurt salts killed those industries which extracted potash from other sources, so did the separation of iodine from the caliche mother-liquors threaten the industrial extraction of iodine from seaweed with extinction. Iodine in a very crude form was exported from Chili in 1874—e.g. a sample was reported with iodine 52-5 per cent. iodine chloride, 3-3 sodium iodate, 13 potassium and sodium nitrate and sulphate, 15 9 magnesium chloride, 0 4 insoluble matter, 1 5 water, 25-2 per cent. About that time much of the iodine was imported as cuprous iodide. This rendered necessary the purification of the Chilian product but now the iodine is purified in Chili before it is exported. The capacity of the Chilian nitre works for the extraction of iodine is greater than the world s demand. It is said that the existing Chilian factories could produce about 5100 tons of iodine per annum whereas the... 

To a solution of N-methyl-4-nitrophenethylamine (1.5 g) (J.O.C., [1956], 21, 45) and 2-[4-nitrophenoxy]ethyl chloride (1.55 g) (C.A., [1955], 49, 3163e) in acetonitrile (50 ml) was added potassium carbonate (1.25 g) and sodium iodide (1.2 g) and the suspension was stirred at reflux for 72 hours. After evaporation to dryness, the residual oily solid was partitioned between a 2 N aqueous sodium bicarbonate solution and ethyl acetate. After two further extractions with ethyl acetate, the organic portions were combined, washed with a saturated aqueous brine solution, dried over magnesium sulfate, filtered and evaporated. The resultant orange solid (2.7 g) was crystallised from ethanol to give l-(4-nitrophenoxy)-2-[N-methyl-N-(4-nitrophenethyl)amino]ethane (1.9 g), m.p. 74°C. 

Now that we have run through the two simple processes. Its time to move onto something a little more advanced. To review what we have learned so far, look at the two similarities between the two procedures we have done. In the first procedure we made ferrous chloride by electrolyzing a salt solution using an iron anode. In the second procedure we used a copper anode, and got cupric chloride. Now, you should remember that if we replaced the copper anode with zinc for example, we would get zinc chloride. Note Any metal can be used with the exception of lead, platinum, and a few others we need not discuss at this point. If you want, try it with aluminum, zinc, nickel, chromium, or magnesium to get the respective chlorides. Note The sodium chloride can be replaced with sodium bromide, or sodium iodide to make the corresponding bromides and iodides. 

Sodium chloride Sodium bromide Sodium iodide Sodium sulphate Sodium silicate Potassium sulphate Lithium chloride Calcium carbonate Calcium sulphate Magnesium sulphate Manganous carbonate Ferrous carbonate. Aluminium phosphate Ammonium nitrate Organic matter... 

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