HRID1796635
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
- -10 °C
PROCEDURE
实验过程
34% H2O2 (53 μl, 0.058 mmol) was added to CH2Cl2 (3 ml) at −10° C., then BF3.Et2O (0.64 ml, 5.0 mmol) was added. After the mixture was stirred at −10° C. for 20 min, a suspension of 396 (165 mg, 0.42 mmol) in CH2Cl2 (2 ml) was added. The reaction was stirred at −10° C. for 5 min, then quenched with aq Na2SO3, extracted with EtOAc. The organic layer was dried, concentrated and purified by silica gel flash column chromatography to give 397A (125 mg, 85%) (10% EtOAc—CH2Cl2).
WORKUP
后处理
- additionwas added
- stirringThe reaction was stirred at −10° C. for 5 min
- customquenched with aq Na2SO3
- extractionextracted with EtOAc
- customThe organic layer was dried
- concentrationconcentrated
- custompurified by silica gel flash column chromatography