反应 #3712070
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05164524
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: The reactions, as illustrated in equations (1), (1)(a), (2), (2)(a), or (2)(b) above, for the production of tetraorganyl tellurium, tetramethyl tellurium, tetraorganyl tellurium, tetra(trimethylsilylmethyl) tellurium, or tetravinyl tellurium, are commenced at low temperature ranging from about -100° C. to about 25° C. If the above reactions are carried out at higher temperature, the corresponding diorganyl tellurium, dimethyl tellurium, bis(trimethylsilyl-methyl) tellurium, or divinyl tellurium derivatives will also be produced, or other side reactions will occur. After the reactions have proceeded to form the tetraorganyl tellurium, tetramethyl tellurium, tetra(trimethylsilylmethyl) tellurium, or tetravinyl tellurium product, the reaction mixture is warmed to room temperature and is stirred; and if a Grignard reagent was used, 1,4-dioxane is added to remove magnesium salts. The slurry is then cooled down again within the above noted -100° C. to 25° C. range, so that all of the salts will precipitate out of solution. The reaction mixture is then filtered to remove precipitated salts. The resulting solution containing the tetraorganyl tellurium, tetramethyl tellurium, tetra(trimethylsilylmethyl) tellurium, or tetravinyl tellurium is then vacuum distilled to remove the solvent, and the crude product purified, e.g., by vacuum distillation for the liquid product,tetramethyl tellurium, or by fractional recrystallization for the solid product, tetra(trimethylsilylmethyl) tellurium. ranging from about -100° C. to about 25° C
来源 ID: ord-4220b9724f2b4ea1be43858a37c83033