HRID17320

反应详情

EQUATION

反应方程式

HRID 17320 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

4-Dimethylaminopyridine (149 mg, 1.22 mmol) was added to a pyridine (100 ml) suspension of 2-(2,2-dimethylpropionylamino)-4-fluoro-5-iodo-3-methoxy-6-methylbenzamide (I-68) (4.97 g, 1.22 mmol), and cooled at 0° C. Trifluoromethanesulfonic acid anhydride (6.17 ml, 36.5 mmol) was dropwise added to it, followed by stirring at room temperature for 1 hour, then ethyl acetate (400 ml) was put thereinto. The organic layer was washed with 1 N hydrochloric acid (300 ml×5), saturated brine (300 ml×2), then dried over anhydrous magnesium sulfate, concentrated under reduced pressure, the residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=5:1) to obtain the entitled compound (4.47 g, 94%) as a pale yellow solid.

WORKUP

后处理

  1. washThe organic layer was washed with 1 N hydrochloric acid (300 ml×5), saturated brine (300 ml×2)
  2. dry with materialdried over anhydrous magnesium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customthe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=5:1)