Pyrex reaction iodides

In the reaction between trifluoromethyl iodide and selenium at 265—290° bistrifluoromethyl selenide, (CF3)2Se, and bistrifluoromethyl diselenide, (CF3)2Sea, are produced in yields of 40 and 20% respectively (Table 4). These two compounds show a number of interesting reactions. The compound (CF3)2Se is converted quantitatively to CF3CI and, SeCl4 when irradiated in a quartz vessel with ultraviolet light. If the irradiation is done in Pyrex, however, a new solid compound CFjSeClg is formed, which hydrolyses to the crystalline acid CF3SeO(OH) (m.p. 118°). The... 

The reaction was studied at nitric oxide and hydrogen iodide pressures of 40-500 and 120-750 torr, respectively. The reaction rate was determined by analyzing for NO and I2 at various times and, in some cases, for ammonium iodide and hydrogen iodide. In clean Pyrex vessels results were not reproducible, but in vessels seasoned with a carbonaceous deposit reproducibility was satisfactory and the reaction was observed to be homogeneous. The rate law was determined to be second order... 

A small scale sulphur iodine process loop made of Pyrex glass was built and operated. The sulphuric acid section and Bunsen reaction section was operated successfully in 2006. In 2008, hydrogen iodide decomposition aided by electro-dialysis (EED) (Hong, 2007) was demonstrated to produce 3.5 litres per... 

A regioselective iodoperfluoroalkylation of terminal alkynes (R—C = CH) has been reported, and is based on photolysis ofthe C—I bond in perfluoroalkyl iodides (Rp-I). Addition of the thus-formed RF" radical onto the alkyne afforded a vinyl radical that in turn abstracts an iodine atom from the starting Rp—I to form the end olefin R-C(I)= CH-Rf. A xenon lamp through Pyrex (hv > 300 nm) was used for the reaction, where aliphatic alkynes gave a better alkylation yield with respect to phenylacetylene [81],... 

In a typical small-scale experiment, trimethylphosphane (l.OOg. 13 mmol) was scaled in a 40-mL Pyrex tube with trifluoroiodomethane (1 4.88 g, 25 mmol), A white crystalline solid was rapidly formed below the surface of the liquid as soon as the temperature approached that of the room, and the reaction was substantially complete within 30 min. The volatile products were removed after 17 h and fractionated in vacuo, logivediniethyl(trifluoromethyl)phosphane(6) yield 0.85 g(5()%). trifluoromcthanc yield 0.032 g, (2% based on trifluoroiodomethane), and trifluoroiodomethane yield 3.46 g (71 V ). The residual solid was identified as tctramethylphosphonium iodide (7) yield 1.46 g (50%) by comparison of its infrared spectrum with that of a sample prepared from trimethylphosphane and methyl iodide. 

The reaction of nitric oxide with hydrogen iodide has been examined by Holmes over the temperature range 360-570 °K. The results in clean pyrex vessels were not reproducible but in vessels with the walls coated with a carbonaceous deposit reproducibility was satisfactory. For the reaction... 

The cylindrical separatory funnel A has a volume of 1200 cc. and holds 2 kg. (15.75 gram atoms) of iodine crystals (Note 2). A piece of perforated platinum foil B, or a loose plug of glass wool, is placed in the bottom to prevent clogging of the stopcock by iodine crystals or solid impurities. Stopcock C is as large as 5 mm. in bore as a further precaution. For the production of up to 4 kg. of methyl iodide, a 5-I. round-bottomed Pyrex flask D is used (Note 3). It is partly submerged in a water bath. Tube E, fitted into the reaction flask by a rubber stopper, is at least 2.5 cm. in internal diameter in order to allow the vapor to rise without interrupting the return of the excess distillate. Tube F is 4 cm. in diameter to allow for preliminary condensation. A space (13 cm.) is left above stopcock G as a reservoir for the distillate. Stopcock G has a bore of 2 or 3 mm. (Note 4). The bottom of the tube from this stopcock is flush with the bottom of the rubber stopper to the iodine container, so that thok ... 

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