HRID396108
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
Trimethylchlorosilane (20.5 g, 190 mmol) is dissolved in 30 mL of tetrahydrofuran. The solution is suspended with sodium (6.50 g, 283 mmol) and then refluxed at 80° C. Under the argon atmosphere, trimethylsilylacetate (3.12 g, 23.6 mmol) in 20 mL of tetrahydrofuran is added via a syringe for an hour and then the solution is refluxed for another 30 minutes. Then, precipitated inorganic residue is filtered and solvent is removed under vacuum. Remained oil is separated by vacuum distillation to give 1,1-bis(trimethylsilyl)ethanol (yield: 55%). b.p. 110° C. (24 mmHg).
WORKUP
后处理
- temperaturethe solution is refluxed for another 30 minutes
- customThen, precipitated inorganic residue
- filtrationis filtered
- customsolvent is removed under vacuum
- customRemained oil is separated by vacuum distillation