HRID2073775

反应详情

EQUATION

反应方程式

HRID 2073775 的结构方程式

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a stirred suspension of 14.7 g 2-chloro-6-methoxy-3-quinolinecarbonitrile in 465 ml absolute ethanol was added 17 ml of hydrazine hydrate. The mixture was stirred at reflux for 24 hours and then cooled to 0° C. The resulting solid product was collected by filtration and boiled with 200 ml water to remove any hydrazine dihydrochloride present. The resulting material was filtered and dried in vacuo (90° C.), and recrystallized from 300 ml dimethylformamide to give 12.3 g 6-methoxy-1H-pyrazolo[3,4-b]quinolin-3-amine as a bright-yellow solid, m.p. >300° C.

WORKUP

后处理

  1. temperatureat reflux for 24 hours
  2. filtrationThe resulting solid product was collected by filtration
  3. customto remove any hydrazine dihydrochloride present
  4. filtrationThe resulting material was filtered
  5. customdried in vacuo (90° C.)
  6. customrecrystallized from 300 ml dimethylformamide