反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
To a solution of 2.59 g of 3-pyridinecarboxaldehyde and 62 mg of tetra-n-butylammonium bromide in 60 mL CH2Cl2 at room temperature is added a solution of 10.0 g of trimethylsulfonium methylsulfate in 15 mL H2O. The resulting solution is set stirring and cooled to 0° C. Aqueous NaOH (50% w/w; 40 mL) is added in portions while stirring and the mixture subsequently refluxed for 1 h. After cooling to room temperature, the mixture is filtered and the filtrate extracted with CH2Cl2. The combined extracts are dried over MgSO4, filtered, and concentrated to yield a red oil, which is subjected to Kugelrohr distillation under high vacuum at 150° C. to yield 838 mg of the title compound as a clear, light yellow oil.
WORKUP
后处理
- stirringwhile stirring
- temperaturethe mixture subsequently refluxed for 1 h
- temperatureAfter cooling to room temperature
- filtrationthe mixture is filtered
- extractionthe filtrate extracted with CH2Cl2
- dry with materialThe combined extracts are dried over MgSO4
- filtrationfiltered
- concentrationconcentrated
- customto yield a red oil, which
- distillationis subjected to Kugelrohr distillation under high vacuum at 150° C.