有機スズ化合物に関する研究(第2報)グリニヤール反応によるフェニルスズ化合物の合成

概要

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The present research was undertaken with the object of preparing triphenyltin compound (an agricultural fungicide) by the Grignard reaction. It has been found that, under suitable conditions, triphenyltin chloride is predominantly produced by the reaction of phenylmagnesium chloride with stannic chloride, thereby tetraphenyltin and diphenyltin compound being obtained only in relatively small amounts.　A typical preparation of this compound was carried out as follows : Stannic chloride (3.3 moles), as a complex compound with tetrahydrofuran (6.6moles), was gradually added to the Grignard reagent (1mole) over an hour period at128 - 133℃, and then the reaction mixture was heated at 140 ℃ for 3 hours. The working-up of the reaction products gave triphenyltin chloride (65.2% yield, based on stannic chloride), tetraphenyltin (12.8%), and diphenyltin compound (9.1%). The Grignard reagent used in this reaction was prepared using xylene as solvent, and tetrahydrofuran and aluminium isopropoxide as catalysts (96% yield, based on magnesium).　Moreover, a satisfactory method for separating the above-described phenyltin compounds from one another was developed.
山形大学の論文
1966-01-14