HRID2213095

反应详情

EQUATION

反应方程式

HRID 2213095 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 2-bromo-5-nitroanisole (5.8 g, 25 mmol) in THF (50 mL) was treated with 2-pyridyl-zinc bromide (50 mL of a 0.5M solution in THF, 25 mmol) and Pd(PPh3)4 (1.44 g, 1.25 mmol). The reaction mixture was degassed by bubbling argon through the solution for min and was subsequently heated to reflux for 12 h while under an atmosphere of argon. The cooled reaction mixture was concentrated and purified by flash column chromatography on silica gel eluting with EtOAc:hexanes (1:19 to 2:3) to afford the desired 2-(2-methoxy-4-nitrophenyl)pyridine.

WORKUP

后处理

  1. customThe reaction mixture was degassed
  2. customby bubbling argon through the solution for min
  3. temperaturewas subsequently heated
  4. temperatureto reflux for 12 h while under an atmosphere of argon
  5. customThe cooled reaction mixture
  6. concentrationwas concentrated
  7. custompurified by flash column chromatography on silica gel eluting with EtOAc:hexanes (1:19 to 2:3)