HRID2073775
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperatureat reflux for 24 hours
- filtrationThe resulting solid product was collected by filtration
- customto remove any hydrazine dihydrochloride present
- filtrationThe resulting material was filtered
- customdried in vacuo (90° C.)
- customrecrystallized from 300 ml dimethylformamide