HRID2213095
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
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
- customThe reaction mixture was degassed
- customby bubbling argon through the solution for min
- temperaturewas subsequently heated
- temperatureto reflux for 12 h while under an atmosphere of argon
- customThe cooled reaction mixture
- concentrationwas concentrated
- custompurified by flash column chromatography on silica gel eluting with EtOAc:hexanes (1:19 to 2:3)