反应详情

温度

150 °C

1,5-Dimethyl-6-methylene-1,6-dihydro-pyridine-3-carboxylic acid (2-benzylamino-4-fluoro-phenyl)-amide I-12′ (186.000 mg; 0.509 mmol) is dissolved in acetic acid and stirred at 150° C. for 1 h in the microwave. The reaction mixture is then concentrated under reduced pressure and 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 product is then dissolved in acetonitrile:water 1:1 and freeze dried.

1. concentrationThe reaction mixture is then concentrated under reduced pressure
2. custompurified 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)
3. additionThe product containing fractions
4. concentrationconcentrated
5. dissolutionThe product is then dissolved in acetonitrile:water 1:1
6. customfreeze dried