Copper iodide purification

The aqueous solution of EtOH was deoxygenated by helium bubbling in the solution for 10 min before use. Methyl vinyl ketone (from Aldrich) was distilled under 20 torr and collected in a round-bottom flask cooled in a C02-acetone bath, immediately before use. Purifications of copper iodide (from Merck, Darmstadt, Germany) and Zn dust (60 fim... 

The CuInS2/ZnS core/shell dots were synthesised by the reaction of indium acetate and copper iodide in octadecene and dodecanthiol at 210 After the synthesis of CuInS2 cores, the shell formation steps were conducted without intermediate purification by addition of zinc stearate and dodecanthiol into CuInS2 core solution. Then the mixed solution was heated to 220 °C and maintained for 7 hours. The final solution was purified using centrifugation and stored in hexane. 

In a dry flask, copper iodide (0.13 mmol) and the ligand 155 (0.54 mmol) are suspended in diethyl ether (13 mL). The suspension is stirred 20 min at 25 °C and then cooled to -78 °C. n-Butylmagnesium chloride (2.0 mmol, solution in diethyl ether) is added, and the mixture stirred for 15 min before a solution of 2-cyclohexenone (156 1.7 mmol) in diethyl ether (4 mL) is dropwise added over 20 min. The reaction mixture is stirred 20 min at -78 °C and worked up in the usual manner. Purification by column chromatography (CH2Cl2/hexane 4 1) followed by short-path distillation afford (-)-(S)-3-butylcyclohexanone (157 92%, 90% ee). The enantiomeric excess is determined by C NMR analysis of the corresponding diastereomeric ketals prepared with (R,R)-2,3-butandiol. ... 

Dimethylphenylsilyl lithium (1 mmol, above THF solution) was added to copper(i) iodide (0.5 mmol) at — 23 °C, and the mixture was stirred at this temperature for 4h. The enone (0.75-0.5mmol) was then added, and stirring was continued at —23 °C for 0.5 h. The mixture was then poured on to ice(25 g)/HCl(5 ml), and extracted with chloroform (3 x 25 ml). The combined extracts were filtered, washed with HCI (25ml, 3m), water (25 ml), saturated sodium hydrogen carbonate solution (25 ml) and water (25 ml), and dried. Concentration and purification by preparative t.l.c. (eluting solvent 3 7 ether petrol) gave the /J-silylketone (40-99%). 

Cyclohexene, purification of, 41, 74 reaction with zinc-copper couple and methylene iodide, 41, 73 2-CyclohEXENONE, 40,14 Cydohexylamine, reaction with ethyl formate, 41, 14... 

Methylene iodide was obtained from Lancaster Synthesis, Inc., and used without further purification. Distillation of the methylene iodide from copper prior to use does not lead to increased product yield or purity. 

Copper(I) iodide purchased from Wako Chemicals was used without purification. 

The excess of copper cyanide and the use of a polar, high-boiling point solvent makes the purification of the products difficult. In addition, elevated temperatures (up to 200°C) lower the functional group tolerance. The use of alkali metal cyanides or cyanation reagents such as cyanohydrins, a catalytic amount of copper(I) iodide and kalium iodide, allows a mild, catalytic cyanation of various aryl bromides. 

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