HRID1196138
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
1 g (3.4 mmol) of 2,3-difluoronaphthacene-5,12-dione, 0.94 g (6.8 mmol) of potassium carbonate, 3.24 g of methanol and 20 ml of tetrahydrofuran (THF) are stirred at 25° C. for 18 hours and under reflux for 3 days. The mixture is cooled and dilute hydrochloric acid is added. The product is filtered off, washed with water, dried and chromatographed with methylene chloride on silica gel. Sublimation under 1.3×10-1 bar/180°-310° C. gives 0.26 g (25%) of pure product, melting point >250° C.
WORKUP
后处理
- temperatureunder reflux for 3 days
- temperatureThe mixture is cooled
- filtrationThe product is filtered off
- washwashed with water
- customdried
- customchromatographed with methylene chloride on silica gel