HRID1052101
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
- 90 °C
PROCEDURE
实验过程
To 1-(5-(benzyloxy)-1H-indazol-3-yl)ethanone (3.50 g, 13.1 mmol) in CH3CN (100 mL) was added K2CO3 (4.54 g, 32.9 mmol) and methyl 2-bromoacetate (1.33 mL, 14.5 mmol). The reaction mixture was stirred at 90° C. for 90 min. Then was filtered and the residue was washed with CH3CN. Volatiles were evaporated and the crude mixture was purified by flash column chromatography on silica gel (c-hexane/EtOAc 1:1 to 1:3). TLC, Rf (c-hexane/EtOAc 1:3)=0.64; MS (LC/MS): 339.0 [M+H]+, 361.0 [M+Na]+; tR (HPLC conditions e): 5.09 min.
WORKUP
后处理
- filtrationThen was filtered
- washthe residue was washed with CH3CN
- customVolatiles were evaporated
- customthe crude mixture was purified by flash column chromatography on silica gel (c-hexane/EtOAc 1:1 to 1:3)
- custom5.09 min.