HRID1093184

反应详情

EQUATION

反应方程式

HRID 1093184 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of N-(4-cyano-1-isopropyl-1H-pyrazol-5-yl)-4-nitrobenzamide (1.3 g, 4.3 mmol) in 1 M aqueous sodium hydroxide solution (9 mL) was made into a homogeneous mixture by the addition of approximately 40 mL of ethanol. Aqueous hydrogen peroxide solution (30%, 5 mL) was added and the mixture was slowly heated to reflux, at which state it remained overnight. After the mixture was allowed to cool to room temperature, it was treated with concentrated hydrochloric acid (5 mL), precipitating a light yellow solid. The solid was collected via Buchner filtration, washed with water, and dried under house vacuum to provide 1-isopropyl-6-(4-nitrophenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-ol as a pale yellow solid (0.76 g, 58%). MS (ES+): 299.8 (M+H)+

WORKUP

后处理

  1. temperaturethe mixture was slowly heated
  2. temperatureto reflux, at which state it
  3. customprecipitating a light yellow solid
  4. filtrationThe solid was collected via Buchner filtration
  5. washwashed with water
  6. customdried under house vacuum