The Activated Method for Zinc Powder
Method 1: Zn powder (100 g) and water (0.9 L) were placed into
a 1-L Erlenmeyer flask equipped with a stir bar. Concd HCl (10 mL)
was added with stirring over 1 min. The slurry was stirred for 20
min and the water was decanted. The metal was washed with water
(3 × 250 mL), acetone (3 × 150 mL), and Et2O (2 × 100 mL). The
metal was then transferred to a flask equipped with a vacuum take-
off and dried under full vacuum for 3 h.
Method 2: In a flame-dried round-bottom flask fitted with magnet-
ic stir bar, dropping funnel, and N2 inlet, zinc powder was placed
and the flask was flushed with anhyd N2. Then 1,2-dibromoethane
(0.1 mL, 2 mL THF) was added and the reaction mixture was heated
to 65 °C until the solvent began to reflux. A few minutes (ca 2 min)
later it was cooled and trimethylchlorosilane (0.1 mL, 1 mL THF)
was added. The solution was stirred at r.t. for 15 min and the organic
solvent was evaporated.
ref Synthesis 2005, No. 17, 2838–2844,
请尽量讲解得详细点!谢谢了!
稀盐酸搅拌 然后乙醚洗两次
加入1 mol/L 的盐酸,
室温下搅拌一会后过滤。
固体在用丙酮洗,油泵抽干就能用了
如果加入盐酸会不会产生大量气泡,而且会很剧烈啊?过滤抽干了,会不会都吸附在滤纸上?谢谢了!
当然会产生气泡了!采用玻璃真空漏斗可以减少吸附
The Activated Method for Zinc Powder
Method 1: Zn powder (100 g) and water (0.9 L) were placed into
a 1-L Erlenmeyer flask equipped with a stir bar. Concd HCl (10 mL)
was added with stirring over 1 min. The slurry was stirred for 20
min and the water was decanted. The metal was washed with water
(3 × 250 mL), acetone (3 × 150 mL), and Et2O (2 × 100 mL). The
metal was then transferred to a flask equipped with a vacuum take-
off and dried under full vacuum for 3 h.
Method 2: In a flame-dried round-bottom flask fitted with magnet-
ic stir bar, dropping funnel, and N2 inlet, zinc powder was placed
and the flask was flushed with anhyd N2. Then 1,2-dibromoethane
(0.1 mL, 2 mL THF) was added and the reaction mixture was heated
to 65 °C until the solvent began to reflux. A few minutes (ca 2 min)
later it was cooled and trimethylchlorosilane (0.1 mL, 1 mL THF)
was added. The solution was stirred at r.t. for 15 min and the organic
solvent was evaporated.
ref Synthesis 2005, No. 17, 2838–2844,