反应详情

A 3-neck 500 mL flask was filled with magnesium turnings (8 g), THF (100 g) and tetraethoxygermane (35 g), and heated to reflux. Crude 2-bromothianthrene (30 g) from Example 1 was added to the flask in small portions. Grignard started after a few minutes and kept refluxing by its own heat for ten minutes. The reaction was allowed to cool for 1 hour, after which magnesium salts were precipitated with heptanes (300 mL). The solution was filtered, followed by evaporation of volatiles by rotary evaporator. The material was distilled three times at <1 mbar, giving colorless 2-(triethoxygermyl)-thianthrene (bp. 180 . . . 210° C., 11 g, 30.5% overall yield based on 2-bromothianthrene, purity 99.5% by GC/MS). FIG. 8 shows the mass spectrum of the compound.

1. temperatureheated to reflux
2. waitGrignard started after a few minutes
3. temperaturekept refluxing by its
4. temperatureown heat for ten minutes
5. temperatureto cool for 1 hour
6. customafter which magnesium salts were precipitated with heptanes (300 mL)
7. filtrationThe solution was filtered
8. customfollowed by evaporation of volatiles by rotary evaporator
9. distillationThe material was distilled three times at <1 mbar