HRID2042637

反应详情

EQUATION

反应方程式

HRID 2042637 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a 500 mL round bottom flask ethyl 2-pyridylacetate (2.0 g, 12.1 mmol), and 60% sodium hydride (508 mg, 12.7 mmol) in dimethylformamide (50 mL) was stirred 1 h. 2-Bromo-1-[4-(3-chloro-propoxy)-phenyl]-ethanone (3.53 g, 12.1 mmol) was then added in dimethylformamide (50 mL) via dropping funnel. The reaction was stirred 14 h. Water (300 mL) was added and the organics were extracted three times with ethyl acetate, and then dried over MgSO4. Purification with silica gel chromatography eluting with hexanes/ethyl acetate (3:1) produced 2.8 g (62%). MS m/z 376 (M+H).

WORKUP

后处理

  1. extractionthe organics were extracted three times with ethyl acetate
  2. dry with materialdried over MgSO4
  3. customPurification with silica gel chromatography
  4. washeluting with hexanes/ethyl acetate (3:1)
  5. customproduced 2.8 g (62%)