HRID1042121

反应详情

EQUATION

反应方程式

HRID 1042121 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A mixture of 5-fluoro-2-nitrophenol (100 g), tetrahydro-2H-pyran-4-yl methanesulfonate (172 g) and potassium carbonate (176 g) in N,N-dimethylformamide (1000 mL) was stirred at 50° C. for 3 days. Water was added to the reaction solution, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over magnesium sulfate, filtered and concentrated under reduced pressure. The obtained crude product was subjected to silica gel column chromatography (ethyl acetate:hexane=0:100 to 25:75, volume ratio) to give the title compound (138 g, yield 90%) as a yellow solid.

WORKUP

后处理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with saturated brine
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe obtained crude product