HRID352822

反应详情

EQUATION

反应方程式

HRID 352822 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl bromo(pyridin-4-yl)acetate hydrochloride (2.05 g) was dissolved in N,N-dimethylformamide (10 ml) at room temperature, followed by the addition of sodium azide (1.43 g). The resulting mixture was stirred for 30 minutes. After the addition of water and stirring, the insoluble matter was filtered off and the filtrate was concentrated. The residue was extracted with diethyl ether and saturated aqueous NaCl solution. The organic layer thus obtained was dried over anhydrous magnesium sulfate. The filtrate was concentrated and the residue was crystallized from methylene chloride, whereby the title compound (yellow powder, 300 mg) was obtained.

WORKUP

后处理

  1. stirringstirring
  2. filtrationthe insoluble matter was filtered off
  3. concentrationthe filtrate was concentrated
  4. extractionThe residue was extracted with diethyl ether and saturated aqueous NaCl solution
  5. customThe organic layer thus obtained
  6. dry with materialwas dried over anhydrous magnesium sulfate
  7. concentrationThe filtrate was concentrated
  8. customthe residue was crystallized from methylene chloride, whereby the title compound (yellow powder, 300 mg)
  9. customwas obtained