HRID963321

反应详情

EQUATION

反应方程式

HRID 963321 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of sodium hydride (70 mg, 2.8 mmol) and 3-hydroxypyridine (0.24 g 2.56 mmol) in DMF was added dropwise 1 g (1g, 2.8 mmol) of 4-(5-methyl-1,2,4-oxadiazol-3-yl)-2,6-dimethyiphenoxypropyl iodide in DMF, and the mixture was stirred at room temperature for 2 days. The mixture was washed with water, extracted with ethyl acetate, and the organic layer was washed with water and dried over magnesium sulfate. The dry organic layer was concentrated in vacuo, passed through a pad of silica gel eluting with hexane/ethyl acetate (1:1) to afford 0.48 g (55.1% of 3-[3-[4-(5-methy-1,2,4-oxadiazol-3-yl) -2,6-dimethylphenoxy]propyl]-pyridine, as an oil, which crystallized on standing in ether, m.p. 46°-49° C.

WORKUP

后处理

  1. washThe mixture was washed with water
  2. extractionextracted with ethyl acetate
  3. washthe organic layer was washed with water
  4. dry with materialdried over magnesium sulfate
  5. concentrationThe dry organic layer was concentrated in vacuo