HRID251825

反应详情

EQUATION

反应方程式

HRID 251825 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 3-(imidazo[1,2-b]pyridazin-2-yl)benzoic acid (1 mmol), DPPA (3 mmol) and Et3N (3 mmol) in toluene was heated to reflux for 4 h. Then t-BuOH (1 ml) was added and reflux was continued overnight. Water was added, and the mixture was extracted with EtOAc. The organic layer was washed with diluted HCl, brine and NaHCO3 (aq), and was concentrated to give a solid. After purification by chromatography, tert-butyl 3-(imidazo[1,2-b]pyridazin-2-yl)phenylcarbamate was obtained with a yield of 38.5%.

WORKUP

后处理

  1. temperatureto reflux for 4 h
  2. temperaturereflux
  3. extractionthe mixture was extracted with EtOAc
  4. washThe organic layer was washed with diluted HCl, brine and NaHCO3 (aq)
  5. concentrationwas concentrated
  6. customto give a solid
  7. customAfter purification by chromatography