HRID2067194

反应详情

EQUATION

反应方程式

HRID 2067194 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-(3-chloro-propoxy)-tetrahydro-pyran (6.28 g, 35.2 mmol), NaN3 (11.4 g, 176 mmol) and potassium iodide (584 mg, 3.52 mmol) in DMF (50 mL) was stirred at RT for 18 h. The reaction mixture was poured into a mixture of Et2O/water. The organic phase was washed with water, brine and then dried (MgSO4), filtered and concentrated in vacuo to give the crude product. The crude product was purified by continuous gradient flash chromatography using EtOAc/petroleum ether (40-60) 0:100 to 15:85 as the eluent to afford the title compound as colourless oil.

WORKUP

后处理

  1. washThe organic phase was washed with water, brine
  2. dry with materialdried (MgSO4)
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customto give the crude product
  6. customThe crude product was purified by continuous gradient flash chromatography