HRID1796635

反应详情

EQUATION

反应方程式

HRID 1796635 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionwas added
  2. stirringThe reaction was stirred at −10° C. for 5 min
  3. customquenched with aq Na2SO3
  4. extractionextracted with EtOAc
  5. customThe organic layer was dried
  6. concentrationconcentrated
  7. custompurified by silica gel flash column chromatography