HRID524428

反应详情

EQUATION

反应方程式

HRID 524428 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

2-(4-cyclopropylsulfonylphenyl)-2-(2,4-difluorophenoxy)acetic acid (Preparation 1; 2.0 g, 5.42 mmol) was dissolved in DCM (20 mL). To this solution was added DMF (0.41 mL, 5.42 mmol) and cooled to 0° C., followed by the addition of oxalyl chloride (0.77 mL, 8.14 mmol) and further stirred for 1 hr at room temp. To this mixture, a solution of tert-butyl 6-aminopyridine-3-carboxylate (preparation 54, 1.26 g, 6.51 mmol) and pyridine (2.19 mL, 2.71 mmol) in DCM 20 (mL) was added drop wise at 0° C. and was stirred further for 1 hr at room temperature. The reaction mixture was diluted with DCM (50 mL), organic layer was washed with water, followed by brine, dried over anhydrous sodium sulfate, solvent was removed under reduced pressure to get the crude compound which was purified by silica gel column chromatography to get the title product (1.6 g).

WORKUP

后处理

  1. stirringwas stirred further for 1 hr at room temperature
  2. washwas washed with water
  3. dry with materialdried over anhydrous sodium sulfate, solvent
  4. customwas removed under reduced pressure
  5. customto get the crude compound which
  6. customwas purified by silica gel column chromatography