9-Bromophenanthrene → 9-(Triethoxygermyl)phenanthrene

関与物質

反応手順

A 3-neck 500 mL flask was filled with magnesium turnings (8 g), THF (100 g) and tetraethoxygermane (35 g), and heated to reflux. 9-Bromophenanthrene (30 g) 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 9-(triethoxygermyl)phenanthrene (bp. 170 . . . 190° C., 21 g, 46.7% overall yield based on 2-bromophenanthrene, purity 99.5% by GC/MS).

情報源と証拠