HRID241796
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 0° C. solution of indanone (1.1 mL, 9.16 mmol, 1.0 equiv) in concentrated H2SO4 (9 mL) was added KNO3 (926 mg, 9.16 mmol, 1.0 equiv) as a solid in several portions over 5 min. After stirring for 1 h, the reaction mixture was poured onto ice. The aqueous suspension was extracted with EtOAC (3×30 mL), and the combined organic layers were washed with brine, dried over sodium sulfate, and concentrated in vacuo. Purification by silica gel chromatography (20%-50% EtOAc/Hexanes) provided the desired compound as a yellow solid (288 mg, 18%).
WORKUP
后处理
- additionthe reaction mixture was poured onto ice
- extractionThe aqueous suspension was extracted with EtOAC (3×30 mL)
- washthe combined organic layers were washed with brine
- dry with materialdried over sodium sulfate
- concentrationconcentrated in vacuo
- customPurification by silica gel chromatography (20%-50% EtOAc/Hexanes)