HRID23712

反应详情

EQUATION

反应方程式

HRID 23712 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

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

  1. stirringwhile stirring
  2. temperaturethe mixture subsequently refluxed for 1 h
  3. temperatureAfter cooling to room temperature
  4. filtrationthe mixture is filtered
  5. extractionthe filtrate extracted with CH2Cl2
  6. dry with materialThe combined extracts are dried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customto yield a red oil, which
  10. distillationis subjected to Kugelrohr distillation under high vacuum at 150° C.