HRID1973027
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
To a solution of 6-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-indazole (0.63 g, 2.56 mmol) in ethyl acetate (7.5 mL) was added triethyloxonium tetrafluoroborate (0.65 g, 3.33 mmol). The mixture was stirred at rt for 5 h under nitrogen (turned to a white suspension after about 0.5 h). The mixture was diluted with ethyl acetate (50 mL) and washed with saturated, aqueous sodium bicarbonate (50 mL). The aqueous layer was extracted with ethyl acetate (2×50 mL), the combined organic layers were dried over MgSO4, filtered and concentrated. The crude purified using an ISCO® instrument using 0-40% ethyl acetate in hexanes. LC-MS [M+H]+=2732, RT=3.27 min.
WORKUP
后处理
- waitturned to a white suspension after about 0.5 h
- washwashed with saturated, aqueous sodium bicarbonate (50 mL)
- extractionThe aqueous layer was extracted with ethyl acetate (2×50 mL)
- dry with materialthe combined organic layers were dried over MgSO4
- filtrationfiltered
- concentrationconcentrated
- customThe crude purified