HRID930519
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
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
1,5-Dimethyl-6-oxo-1,6-dihydro-pyridine-3-carboxylic acid [2-benzylamino-4-(4-methyl-piperazin-1-yl)-phenyl]-amide I-1′ (523.000 mg; 1.174 mmol) is dissolved in acetic acid and stirred at 80° C. overnight. The reaction mixture is concentrated under reduced pressure and the residue is purified on silica chromatography Combiflash (Column: Redisep Rf, 40 g; gradient: DCM/MeOH=100%/0% to 95%/5% over 30 column volumes, then to 90%/10% over 15 column volumes; flow rate=40 ml/min; detection wavelength: 254 nm). Product containing fractions are combined and concentrated under reduce pressure.
WORKUP
后处理
- concentrationThe reaction mixture is concentrated under reduced pressure
- customthe residue is purified on silica chromatography Combiflash (Column
- additionProduct containing fractions
- concentrationconcentrated