HRID1292478
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A mixture of 500 mg of 1H-imidazo[4,5-c]quinolin-4-ol and about 6 mL of phosphorous oxychloride was heated on a steam bath for about 16 hours, then poured over ice. The mixture was neutralized with saturated sodium bicarbonate solution, then the solid was separated by filtration. The solid was dissolved in dilute hydrochloric acid, the mixture was filtered and the filtrate was neutralized with concentrated ammonium hydroxide to reprecipitate the product. Filtration and drying was followed by recrystallization from methanol to provide crystals of 4-chloro-1H-imidazo[4,5-c]-quinoline. Analysis: Calculated for C10 H6N3 : % C, 59.0; % H, 3.0; % N, 20.6; Found: % C, 59.5; % H, 3.0; % N, 20.2.
WORKUP
后处理
- temperaturewas heated on a steam bath for about 16 hours
- additionpoured over ice
- customthe solid was separated by filtration
- dissolutionThe solid was dissolved in dilute hydrochloric acid
- filtrationthe mixture was filtered
- filtrationFiltration
- customdrying
- customwas followed by recrystallization from methanol