2,2,4,4,6,6,8,8-octamethyl-1,3,5,7,2,4,6,8-tetrazatetrasilocane

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The starting octamethylcyclotetrasilazane should effectively be one which is secondarily produced when hexamethylcyclotrisilazane is prepared by reaction between dimethyl dichlorosilane and ammonia. Using such secondarily produced octamethylcyclotetra-silazane, the amount of hexamethylcyclo-trisilazane formed per unit starting material can be maximized. At the same time, some technical problems can be solved including elimination or treatment of octamethylcyclo-tetrasilazane in the form of a solid (melting point of 97° C.) which is left in the distillation column after removal of hexamethylcyclo-trisilazane by distillation.

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The starting octamethylcyclotetrasilazane should effectively be one which is secondarily produced when hexamethylcyclotrisilazane is prepared by reaction between dimethyl dichlorosilane and ammonia. Using such secondarily produced octamethylcyclotetra-silazane, the amount of hexamethylcyclo-trisilazane formed per unit starting material can be maximized. At the same time, some technical problems can be solved including elimination or treatment of octamethylcyclo-tetrasilazane in the form of a solid (melting point of 97° C.) which is left in the distillation column after removal of hexamethylcyclo-trisilazane by distillation.

反応条件: temp:97.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A 200 ml volume glass flask equipped with a stirring machine, a condenser, a distillation column and a tube for distilling off the resulting product was provided. 73 g of octamethyl cyclotetrasilazane and 3.65 g of p-toluidine-m-sulfonic acid as a catalyst were introduced into the glass flask and the content of the flask was heated to 97° C. The content of the flask was stirred after it was confirmed that the octamethyl cyclotetrasilazane was completely molten. When the internal pressure of the reaction system was reduced to 65 torr with a vacuum pump to obtain a distillate, 68 g of hexamethyl cyclotrisilazane was obtained through the distillation over one hour. The resulting hexamethyl cyclotrisilazane had a high purity in the order of 99.1 GC % and the yield thereof was 93.2%. Thus, highly pure hexamethyl cyclotrisilazane could be obtained at a high yield within a short period of time. Moreover, almost no high boiling point substance remained in the reaction system. A 200 ml volume glass flask equipped with a stirring machine, a condenser a distillation column and a tube for distilling off the resulting product was provided to obtain a distillate

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The starting octamethylcyclotetrasilazane should effectively be one which is secondarily produced when hexamethylcyclotrisilazane is prepared by reaction between dimethyl dichlorosilane and ammonia. Using such secondarily produced octamethylcyclotetra-silazane, the amount of hexamethylcyclo-trisilazane formed per unit starting material can be maximized. At the same time, some technical problems can be solved including elimination or treatment of octamethylcyclo-tetrasilazane in the form of a solid (melting point of 97° C.) which is left in the distillation column after removal of hexamethylcyclo-trisilazane by distillation.