HRID922466

反应详情

EQUATION

反应方程式

HRID 922466 的结构方程式

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

to a mixture of 2-chloro-6-methylnicotinaldehyde (5.0 g) and hydrazine monohydrate (6.24 mL) was added para-toluenesulfonic acid monohydrate (3.67 g), and the mixture was stirred at 130° C. for 18 hours. The reaction solution was cooled, and then thereto was added 10% aqueous citric acid solution, and the mixture was stirred at room temperature for 30 minutes. The reaction solution was extracted with ethyl acetate, and washed with saturated saline. The organic layer was dried over sodium sulfate, and then concentrated under reduced pressure to give 6-methyl-1H-pyrazolo[3,4-b]pyridine [REx(104-1)] (3.61 g) as a brown powder.

WORKUP

后处理

  1. temperatureThe reaction solution was cooled
  2. stirringthe mixture was stirred at room temperature for 30 minutes
  3. extractionThe reaction solution was extracted with ethyl acetate
  4. washwashed with saturated saline
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. concentrationconcentrated under reduced pressure