HRID930519

反应详情

EQUATION

反应方程式

HRID 930519 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. concentrationThe reaction mixture is concentrated under reduced pressure
  2. customthe residue is purified on silica chromatography Combiflash (Column
  3. additionProduct containing fractions
  4. concentrationconcentrated