HRID1731296

反应详情

EQUATION

反应方程式

HRID 1731296 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Ethyl 7-chloro-1H pyrazolo[4,3-b]pyridine-6-carboxylate (1.0 g, 0.004 mole) and p-aminophenol (1.0 g, 0.009 mole) were stirred together in ethyl acetate (200 ml) under nitrogen for 48 hours, the temperature being maintained between -10° and -5° C. The ethyl acetate was removed under reduced pressure to give a yellow solid. This solid was dissolved in aqueous ethanol and the pH adjusted to pH8 with 10% sodium carbonate solution. The resulting solid was filtered off washed with water and dried. Recrystallization from methanol/ethyl acetate gave the title compound as a pale yellow solid (650 mg, 50%), m.p. 286°-287° C. (decomposition)

WORKUP

后处理

  1. temperaturethe temperature being maintained between -10° and -5° C
  2. customThe ethyl acetate was removed under reduced pressure
  3. customto give a yellow solid
  4. filtrationThe resulting solid was filtered off
  5. washwashed with water
  6. customdried
  7. customRecrystallization from methanol/ethyl acetate