HRID590773

反应详情

EQUATION

反应方程式

HRID 590773 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

A flask containing 6-chloro-3-iodo-4-methyl-1H-pyrazolo[4,3-c]pyridine (2.06 g, 7.02 mmol) in THF (60 mL) was cooled to 0° C. and potassium hydride (1.126 g, 14.04 mmol) was added. The reaction was stirred for 30 min followed by addition of trityl chloride (2.94 g, 10.53 mmol). The reaction mixture was warmed to room temperature and stirred for 4 h. The reaction was poured into sat. sodium bicarbonate and extracted with EtOAc. The organic phase was dried over MgSO4, filtered, and concentrated in vacuo. The residue was purified by flash chromatography (0-10% DCM/EtOAc) to give 6-chloro-3-iodo-4-methyl-1-trityl-1H-pyrazolo[4,3-c]pyridine. MS ESI calc'd. for C26H19ClIN3 [M+1]+ 536. found 536.

WORKUP

后处理

  1. temperatureThe reaction mixture was warmed to room temperature
  2. stirringstirred for 4 h
  3. extractionextracted with EtOAc
  4. dry with materialThe organic phase was dried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by flash chromatography (0-10% DCM/EtOAc)