HRID2048096

反应详情

EQUATION

反应方程式

HRID 2048096 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

To a solution of 3-chloro-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-2-[(1S)-2,2,2-trifluoro-1-methylethoxy]pyridine (Preparation 232, 130 mg, 0.37 mmol) in acetone (1 mL) was added an aqueous solution of Oxone® (1 mL, 287 mg, 0.44 mmol) dropwise with stirring at 0° C. for 15 minutes. The reaction mixture was diluted with water and extracted with DCM (3×5 mL). The mixture was filtered through a phase separation cartridge, the organic phase was washed with brine (3 mL) and filtered through another phase separation cartridge. The filtrate was dried by N2 blowing to give a crude product that was purified by silica gel column chromatography eluting with 0-30% EtOAc in heptane to give the title compound (62 mg, 69%) as colourless oil.

WORKUP

后处理

  1. extractionextracted with DCM (3×5 mL)
  2. filtrationThe mixture was filtered through a phase separation cartridge
  3. washthe organic phase was washed with brine (3 mL)
  4. filtrationfiltered through another phase separation cartridge
  5. dry with materialThe filtrate was dried by N2 blowing
  6. customto give a crude product that
  7. customwas purified by silica gel column chromatography
  8. washeluting with 0-30% EtOAc in heptane