反应详情

A 3-neck 1 L flask was filled with magnesium turnings (5 g), THF (200 g) and tetramethoxysilane (50 g), and heated to reflux. 2-Bromothianthrene (40 g), prepared analogously to Example 3A was added to the flask in 10 g portions. Grignard started within 10 minutes. The reaction was allowed to cool for 1 hour, after which magnesium salts were precipitated with hexanes (200 mL). GC/MS of the solution showed that along with some thianthrene, 2-(trimethoxysilyl)thianthrene was obtained in ˜60% yield (FIG. 7).

1. temperatureheated to reflux
2. additionwas added to the flask in 10 g portions
3. temperatureto cool for 1 hour
4. customafter which magnesium salts were precipitated with hexanes (200 mL)