HRID251825
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureto reflux for 4 h
- temperaturereflux
- extractionthe mixture was extracted with EtOAc
- washThe organic layer was washed with diluted HCl, brine and NaHCO3 (aq)
- concentrationwas concentrated
- customto give a solid
- customAfter purification by chromatography