HRID2359040

反应详情

EQUATION

反应方程式

HRID 2359040 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

To 2-Chloro-4-[1-sec-butyl-3-(5-chloro-2-thienyl)-1H-pyrazol-4-yl]pyridine (0.57 mmol) was added slowly 0.5 mL of a 33% solution hydrobromic acid in acetic acid. The resulting mixture was stirred in the microwave at 140° C. for 20 min. After cooling to room temperature, potassium carbonate (2 molar solution) was added and the aqueous layer was extracted with ethyl acetate. The organic layers were combined, dried over MgSO4 and evaporated. The residue was purified by chromatography on silica gel (hepthane:ethyl acetate 5:1 to 2:1) to afford 178 mg of 2-bromo-4-[1-sec-butyl-3-(5-chloro-2-thienyl)-1H-pyrazol-4-yl]pyridine (79% yield).

WORKUP

后处理

  1. temperatureAfter cooling to room temperature
  2. extractionthe aqueous layer was extracted with ethyl acetate
  3. dry with materialdried over MgSO4
  4. customevaporated
  5. customThe residue was purified by chromatography on silica gel (hepthane:ethyl acetate 5:1 to 2:1)