HRID53674
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To 10.4 g (0.025 mol) of 8-chloro-[1,3]dioxolo [4,5-g]quinoline-7-carboxylic acid (2-pyridin-2yl-ethyl)-amide in 100 mL of ethanol was added 7.2 g (0.1 mol) of sodium hydrogensulfide and the mixture was heated at reflux for 3 hours. The mixture was cooled and the solids filtered, washed with ethanol, and then with water. The filtrate was concentrated and the solids were suspended in water, collected by filtration, and recrystallized from ethanol to give 6.8 g of the title compound, mp 258°-260° C.
WORKUP
后处理
- temperaturethe mixture was heated
- temperatureat reflux for 3 hours
- temperatureThe mixture was cooled
- filtrationthe solids filtered
- washwashed with ethanol
- concentrationThe filtrate was concentrated
- filtrationcollected by filtration
- customrecrystallized from ethanol