HRID1182345

反应详情

EQUATION

反应方程式

HRID 1182345 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

1.2 L of tetrahydrofuran and 87.8 g (0.78 mole) of potassium t-butoxide were added to a reactor and cooled to 0° C. 71.5 mL (0.74 mol) of methyl propionate was dropwise added to the reactor and stirred at 0° C. for 30 minutes. 60 g (0.434 mole) of the methyl pyrazine-2-carboxylate of Example 1 dissolved in 500 mL of tetrahydrofuran was dropwise added to the reactor for 30 minutes and stirred at a temperature of 20 to 25° C. for 3 hours. 0.5 L of distilled water and 0.5 L of saturated ammonium chloride solution were added to the reaction solution and stirred for 30 minutes. The resultant reaction solution was concentrated to a volume of 1.0 L and then extracted with 1.0 L of methylenechloride. The resultant extract was dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated to give 75.0 g of the titled compound as a dark brown viscous oil (yield 89.0%).

WORKUP

后处理

  1. additionwas dropwise added to the reactor for 30 minutes
  2. stirringstirred at a temperature of 20 to 25° C. for 3 hours
  3. stirringstirred for 30 minutes
  4. customThe resultant reaction solution
  5. concentrationwas concentrated to a volume of 1.0 L
  6. extractionextracted with 1.0 L of methylenechloride
  7. extractionThe resultant extract
  8. dry with materialwas dried over anhydrous magnesium sulfate
  9. filtrationfiltered
  10. concentrationThe filtrate was concentrated