HRID2039612
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 a solution of 1.5 g (6.96 mmol) of 2,4,5-triamino-3-chloro-benzoic acid methyl ester in 27 ml of EtOH, is added 0.81 ml (9.18 mmol) of 2,3-butanedione. The mixture is stirred under reflux during 1 hour. After cooling the mixture to ambient temperature EtOAc is added and the organic phase is washed with H2O (2 times). The organic phase is dried on Na2SO4, filtrated and evaporated. After purification by flash chromatography on silica gel, 1.18 g (4.22 mmol, 62%) of an orange-coloured solid were obtained. 1H-NMR (CDCl3, 300 MHz): ? ppm=2.67 (s, 3H), 2.75 (s, 3H), 3.97 (s, 3H), 6.47 (s br, 2H), 8.58 (s, 1H).
WORKUP
后处理
- temperatureunder reflux during 1 hour
- additionis added
- washthe organic phase is washed with H2O (2 times)
- customThe organic phase is dried on Na2SO4
- filtrationfiltrated
- customevaporated
- customAfter purification by flash chromatography on silica gel