HRID1694528

反应详情

EQUATION

反应方程式

HRID 1694528 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 2,8-dibromoquinoline (4.64 g, 16 mmol, prepared by the method of L. Mao et al., Tetrahedron Lett. 46 (2005) 8419), 3,5-di-tert-butyl-2-methoxyphenylboronic acid (4.3 g, 16 mmol), K2CO3 (5.6 g, 40 mmol), Pd(OAc)2 (0.08 g, 0.3 mmol), P(o-Tol)3 (0.2 g, 0.6 mmol), dimethoxyethane (40 mL) and water (10 mL) is refluxed for 8 h with stirring in an argon atmosphere. The mixture is then poured into water and extracted with CHCl3 (3×50 mL). The combined organic phase is washed with water and brine, and then concentrated. The residue is purified by column chromatography (silica gel 40, hexane/CH2Cl24:1). Yield: 5.2 g (77%).

WORKUP

后处理

  1. customprepared by the method of L
  2. extractionextracted with CHCl3 (3×50 mL)
  3. washThe combined organic phase is washed with water and brine
  4. concentrationconcentrated
  5. customThe residue is purified by column chromatography (silica gel 40, hexane/CH2Cl24:1)