HRID1670539

反应详情

EQUATION

反应方程式

HRID 1670539 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Add pyridinium tribromide (7 g, 22 mmol) to a solution of 5-acetyl-2-bromo-pyridine (4 g, 20 mmol) in THF (100 mL) at room temperature. Stir the mixture for 16 h at ambient temperature under a nitrogen atmosphere. Quench the mixture with saturated aqueous NaHCO3 (50 mL, pH at 7.8). Extract the mixture with EtOAc (150 mL). Wash the organic layer with brine (50 mL) and concentrate in vacuo to obtain the desired intermediate as a dark brown oil (11.5 g) that was used without further purification. MS (ES+) m/z: 280.0 (M+H)+.

WORKUP

后处理

  1. customQuench the mixture with saturated aqueous NaHCO3 (50 mL
  2. extractionExtract the mixture with EtOAc (150 mL)
  3. washWash the organic layer with brine (50 mL)
  4. concentrationconcentrate in vacuo