反应详情

A one liter apparatus similar to that of Example 2 was charged with 162 g tributyltin chloride. During 20 minutes 87.3 ml Reagent T was added while keeping the temperature at 28°-30° C. by using an ice-water bath. The mixture was then heated at 45°-50° C. for 30 minutes and filtered. The filtrate was stripped of toluene under reduced pressure and distilled to give 137.6 g (95% of theoretical yield) tributyltin hydride, boiling 118°-124° C. at 5 to 6 mm. A 15 g portion of the tributyltin hydride was mixed with 26.6 g trimethyltin chloride solution (38.6% in toluene) and distilled immediately. The distillate boiling up to 110° C. weighed 17.9 g and consisted, according to NMR analysis, of 46.8% trimethyltin hydride and 53.2% toluene. Thus the contained trimethyltin hydride (8.5 g) represents a 98.8% of theoretical yield based on trimethyltin chloride and a 93.9% of theoretical yield for the two stages of tributyltin chloride reduction to tributyltin hydride according to this invention and transposition to trimethyltin hydride and tributyltin chloride for recycle to the process. Inclusion of the hydride exchange reaction enables the relatively small losses of organotin species during the reduction step to be borne by the commercially available and less toxic tributyltin, thus economizing and minimizing exposure to the less available trimethyltin.

1. customboiling 118°-124° C. at 5 to 6 mm
2. distillationdistilled immediately
3. customboiling up to 110° C.
4. customof theoretical yield