HRID8259

反应详情

EQUATION

反应方程式

HRID 8259 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of dimethylamino-acetyl chloride (620.0 mg, 13.33 mmol), 4-(2-pyridin-2-yl-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazol-3-yl)-quinolin-7-ylamine (75 mg, 0.23 mmol), and 4-N,N-dimethylaminopyridine (10.2 mg, 0.09 mmol) in dry pyridine (1 mL) is refluxed for 72 h. The mixture is treated with saturated sodium bicarbonate solution and extracted with ethyl acetate. The organic layer is washed with brine, dried (sodium sulfate), concentrated in vacuo, and the residue chromatographed on SiO2 ((5% to 20% methanol in dichloromethane) to yield a yellow oil, 62.3 mg (67%).

WORKUP

后处理

  1. temperatureis refluxed for 72 h
  2. extractionextracted with ethyl acetate
  3. washThe organic layer is washed with brine
  4. dry with materialdried (sodium sulfate)
  5. concentrationconcentrated in vacuo
  6. customthe residue chromatographed on SiO2 ((5% to 20% methanol in dichloromethane)
  7. customto yield a yellow oil, 62.3 mg (67%)