HRID2308241

反应详情

EQUATION

反应方程式

HRID 2308241 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 4-nitro-3-trifluoromethylphenol (27 g, 130 mmol) in acetone (250 mL) was treated with K2CO3 (18 g, 130 mmol) and methyl iodide (16 mL, 260 mmol) and the mixture was heated at reflux under nitrogen. After 16 h, the cooled mixture was filtered to remove K2CO3 and the filtrate was concentrated in vacuo to give the crude product (32 g), which was taken up in benzene (250 mL). The organic solution was washed with water and brine (125 mL each), dried (MgSO4) and concentrated in vacuo to give the title compound (27 g, 94%) as a yellow oil which was pure enough for further use.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureat reflux under nitrogen
  3. filtrationthe cooled mixture was filtered
  4. customto remove K2CO3
  5. concentrationthe filtrate was concentrated in vacuo
  6. customto give the crude product (32 g), which
  7. washThe organic solution was washed with water and brine (125 mL each)
  8. dry with materialdried (MgSO4)
  9. concentrationconcentrated in vacuo