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
CONDITIONS
反应条件
- 温度
- 180 °C
PROCEDURE
实验过程
To a mixture of 6-fluoro-1-(piperidin-4-yl)indoline (128 mg, 0.5 mmol), 3-chloro-6-(4-methylimidazol-1-yl)pyridazine (78 mg, 0.4 mmol) in DMSO (1.5 mL) was added DIPEA (0.25 mL, 1.5 mmol). The resulting mixture was sealed and heated at 180° C. for 1.5 h under microwave irradiation. The resulting mixture was then poured into H2O (30 mL) and the aqueous layer was extracted with 10% CH2Cl2/Et2O (80 mL×4). The combined organic layer was dried (Na2SO4) and filtered. The solvent was removed and the resulting residue was purified by column (dry loading) using EtOAc then 3% MeOH/EtOAc as the eluent to yield 6-fluoro-1-(1-(6-(4-methyl-1H-imidazol-1-yl)pyridazin-3-yl)piperidin-4-yl)indoline.
WORKUP
后处理
- customThe resulting mixture was sealed
- extractionthe aqueous layer was extracted with 10% CH2Cl2/Et2O (80 mL×4)
- dry with materialThe combined organic layer was dried (Na2SO4)
- filtrationfiltered
- customThe solvent was removed
- customthe resulting residue was purified by column (dry loading)