HRID1011861

反应详情

EQUATION

反应方程式

HRID 1011861 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
2 °C

PROCEDURE

实验过程

5.21 g=5.02 ml (39.2 mmol) of 3-oxo-pentanoic acid methyl ester were dissolved in 30 ml of CH2Cl2, the solution was cooled to 2° C. and 3.81 g (39.2 mmol) of anhydrous magnesium chloride were added in small portions. Then, 6.21 g=6.34 ml (78.4 mmol) of pyridine were added to this suspension between 2° C. and 5° C., followed by 3.89 g=3.67 ml (41.2 mmol) of propionyl chloride. The reaction mixture was warmed up to RT and 1 hour later poured into crashed ice, acidified with HCl (25%) to pH 1-2 and extracted twice with Et2O. The organic phases were dried over magnesium sulfate, filtered and evaporated to give 7.62 g of title compound as light yellow oil. MS: 185.1 ([M−H]−).

WORKUP

后处理

  1. temperatureThe reaction mixture was warmed up to RT and 1 hour
  2. additionlater poured
  3. extractionextracted twice with Et2O
  4. dry with materialThe organic phases were dried over magnesium sulfate
  5. filtrationfiltered
  6. customevaporated