HRID1527306

反应详情

EQUATION

反应方程式

HRID 1527306 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 3-iodo-5-methyl-1H-pyrazolo[3,4-c]pyridine (1.00 g, 3.86 mmol), and potassium carbonate (1.28 g, 9.26 mmol) in acetonitrile (40 mL) was added tert-butyl bromoacetate (0.685 mL, 4.63 mmol) dropwise at RT and the resulting mixture was heated to reflux for 16 h. The mixture was cooled to RT and filtered, the solid was washed with acetonitrile and the filtrate was concentrated under vacuum. The residual oil was used directly in the next step without further purification. MS (LC/MS): 374.0 [M+H]+; tR (HPLC conditions k): 2.96 min.

WORKUP

后处理

  1. temperaturethe resulting mixture was heated
  2. temperatureto reflux for 16 h
  3. filtrationfiltered
  4. washthe solid was washed with acetonitrile
  5. concentrationthe filtrate was concentrated under vacuum
  6. customThe residual oil was used directly in the next step without further purification
  7. custom2.96 min.