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
- 140 °C
PROCEDURE
实验过程
To a 10 mL vial was added a mixture of 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-6-(trifluoromethyl)-1H-indazole (0.066 g, 0.211 mmol), methyl 3-bromoimidazo[1,2-b]pyridazine-6-carboxylate (0.054 g, 0.211 mmol) and PdCl2(dppf) (7.74 mg, 10.57 μmol) in dioxane (2 mL) and aqueous saturated NaHCO3 (1 mL). The resulting orange suspension was heated at 140° C. for 30 minutes in a microwave reactor. The major peak by LCMS was the decarboxylated product. The reaction mixture was extracted into EtOAc and the water layer was separated and acidified with concentrated HCl to pH 2. The water layer was extracted with EtOAc. The organic layers were combined, dried over Na2SO4, filtered, and concentrated to give an oil, which was used without further purification (36 mg).
WORKUP
后处理
- additionTo a 10 mL vial was added
- extractionThe reaction mixture was extracted into EtOAc
- customthe water layer was separated
- extractionThe water layer was extracted with EtOAc
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- customto give an oil, which
- customwas used without further purification (36 mg)