HRID930527

反应详情

EQUATION

反应方程式

HRID 930527 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

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