HRID497954

反应详情

EQUATION

反应方程式

HRID 497954 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
180 °C

PROCEDURE

实验过程

A mixture of ethyl 4-hydroxy-3-methyl-1-(2-pyridinyl)-1H-pyrazolo[3,4-b]pyridine-5-carboxylate (2.0 g, 6.7 mmol) and benzylamine (8.0 mL, 73 mmol) was stirred at 180° C. for 16 hours under an argon atmosphere. The mixture was cooled to room temperature, ethyl acetate was added thereto. The resulting crude crystals were collected by filtration, and washed with ethyl acetate. The crude crystals thus obtained were purified by silica gel column chromatography (chloroform:methanol=20:1 to 5:1), and recrystallized from ethanol to give the title compound (1.5 g, 60% yield).

WORKUP

后处理

  1. temperatureThe mixture was cooled to room temperature
  2. filtrationThe resulting crude crystals were collected by filtration
  3. washwashed with ethyl acetate
  4. customThe crude crystals thus obtained
  5. customwere purified by silica gel column chromatography (chloroform:methanol=20:1 to 5:1)
  6. customrecrystallized from ethanol