HRID70712

反应详情

EQUATION

反应方程式

HRID 70712 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

48% hydrobromic acid (3 mL) was added to a solution of 5-cyclopropyl-6-methoxypyridine-2-carbaldehyde obtained in Reference Example 1-51(6) (437 mg) in 1,4-dioxane (6 mL), and the mixture was stirred at 65° C. for two hours. The reaction solution was poured into water, followed by extraction with chloroform/methanol (2:1). The organic layer was dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=75:25→0:100) to give 5-cyclopropyl-6-oxo-1,6-dihydropyridine-2-carbaldehyde as a yellow powder (278 mg, 69%).

WORKUP

后处理

  1. extractionfollowed by extraction with chloroform/methanol (2:1)
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. customThe resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=75:25→0:100)