HRID930527
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
- 150 °C
PROCEDURE
实验过程
1,5-Dimethyl-6-oxo-1,6-dihydro-pyridine-3-carboxylic acid (4-benzylamino-6-morpholin-4-yl-pyridin-3-yl)-amide II-3′ (73.000 mg; 0.168 mmol) is dissolved in acetic acid (2.1 g) and stirred at 150° C. for 10 h in the microwave. The reaction mixture is concentrated under reduced pressure. The residue is purified on silica chromatography Combiflash (Column: Redisep Rf, 12 g; gradient: DCM/MeOH=100%/0% to 90%/10%; flow rate=30 ml/min; 28 column volumes; detection wavelength: 254 nm). The product containing fractions are combined and concentrated under reduce pressure. The residue is then dissolved in acetonitrile:water 1:1 and freeze dried
WORKUP
后处理
- concentrationThe reaction mixture is concentrated under reduced pressure
- customThe residue is purified on silica chromatography Combiflash (Column: Redisep Rf, 12 g; gradient: DCM/MeOH=100%/0% to 90%/10%; flow rate=30 ml/min; 28 column volumes; detection wavelength: 254 nm)
- additionThe product containing fractions
- concentrationconcentrated
- dissolutionThe residue is then dissolved in acetonitrile:water 1:1 and freeze
- customdried