Diethyl ether electrolysis

The colorless crystalline product that accumulates during the electrolysis is collected and can be recrystallized from hot methanol or ethanol (25 mL). The crystals are collected, washed with diethyl ether (2 X 25 mL), and dried in vacuo for 1 hour. Yield 2.8 g (92%). Anal. Calcd. for C6Hlg03S3lnCl3 In, 25.3 C. 23.4 Found In, 25.3 Cl, 23.1. 

The pre-electrolysis of 1 mmol of MesSiCl for about 1.5 h preceded the main electrolysis to eliminate formed fiom hydrolyses of the chlorosilane by residual water. The silanone precursor (50 mmol) and a trap (55 mmol) were then injected into the cell using a syringe, and the electrolysis was continued with constant flow of O2 through the solution (5 mL min ) and the current density j 5 - 7 mA cmT, the cathode potential not to exceed -2 V. From THF and DMF solutions, the products were isolated as described earlier [6, 7] when the process was carried out in IL, thorough extraction with diethyl ether, evaporation of the latter and distillation of the organic residue were effected to isolate the products. 

Dense and clear colorless to yellowish liquid with a pungent odor of chloroform. Quite chemically inert to most minerals. Miscible with ethanol, diethyl ether, acetone, benzene, and carbon tetrachloride. Decomposed when exposed to sunlight and it must be stored in brown inactinic glass bottle. It can be stabilized by adding 2-3 wt.% of ethanol. Solubility in water at 20°C 3.2 g/L. Prepared by electrolysis of sodium bromide and acetone or by reacting sodium hypobromite with acetone ". Highly toxic. 

Step 2 is achieved in the same cdl, immediately after electrolysis. An equimolar amount (10 mmol) of 1,2-dihaloethylene is added to the solution, together with 2mol% of PdCfi(PPhfi2. The solution was stirred and heated at 60 Cfor 12h. After this time, both the arylzinc species and 1,2-dihaloethylene are consumed, which was verified by GC. The reaction mixture was poured into a solution of 6N HCl (50mL) and extracted with diethyl ether (2x25 ml). The combmated extracts were filtered and washed with distilled water, methanol and pentane. 

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