HRID2060914
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
1-Acetyl-4-bromo-1H-indole-3-carbaldehyde (3.5 g, 13.2 mmol) was dissolved in CH2Cl2 (50 mL). 3-Chloroperbenzoic acid (3.9 g, 15.8 mmol) was added, and the reaction stirred 16 h at r.t. The solution was washed with sat. NaHCO3 and brine, dried (MgSO4), and concentrated. The residue was stirred with K2CO3 (100 mg) in MeOH (50 mL) for 2 min. The solution was concentrated and purified by silica gel chromatography (100% CH2Cl2) to provide the title compound as a faintly blue solid (880 mg, 26%). MS (ES) [m+H] calc'd for C10H8BrNO2, 254, 256; found 254, 256.
WORKUP
后处理
- washThe solution was washed with sat. NaHCO3 and brine
- dry with materialdried (MgSO4)
- concentrationconcentrated
- stirringThe residue was stirred with K2CO3 (100 mg) in MeOH (50 mL) for 2 min
- concentrationThe solution was concentrated
- custompurified by silica gel chromatography (100% CH2Cl2)