HRID497950
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 180 °C
PROCEDURE
实验过程
A suspension of 4-hydroxy-3-methyl-1-(2-pyridinyl)-1H-pyrazolo[3,4-b]pyridine-5-carboxylic acid (2.0 g, 6.7 mmol) in phosphoric acid (10 mL) was heated and stirred at 180° C. for 12 hours. The reaction solution was cooled to room temperature, neutralized by the addition of an aqueous sodium hydroxide solution, and organic matter was extracted with chloroform. The extract was washed with saturated brine and water, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. Purification of the residue by silica gel column chromatography (chloroform:methanol=95:5) gave the title compound (230 mg, 15% yield).
WORKUP
后处理
- temperaturewas heated
- temperatureThe reaction solution was cooled to room temperature
- extractionwas extracted with chloroform
- washThe extract was washed with saturated brine and water
- dry with materialdried over anhydrous magnesium sulfate
- customthe solvent was evaporated under reduced pressure
- customPurification of the residue by silica gel column chromatography (chloroform:methanol=95:5)