HRID2115823

反应详情

EQUATION

反应方程式

HRID 2115823 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution/suspension of methyl 6-hydroxy-1-naphthoate (2.49 g, 12.3 mmol), 6-methoxypyridin-3-ylboronic acid (2.26 g, 14.8 mmol), copper acetate (2.46 g, 13.6 mmol), triethylamine (6.24 g, 61.7 mmol) and 4 Å molecular sieves (2.00 g) in acetonitrile (120 mL) was stirred at RT for 16 h. The solids were filtered off. The filtrate was concentrated in vacuo. Water was added and extracted with EtOAc. The organic layer was washed with 1M aqueous NaOH solution, water, brine and dried over Na2SO4, filtered and concentrated in vacuo. Purification by silica gel chromatography afforded the title compound.

WORKUP

后处理

  1. filtrationThe solids were filtered off
  2. concentrationThe filtrate was concentrated in vacuo
  3. additionWater was added
  4. extractionextracted with EtOAc
  5. washThe organic layer was washed with 1M aqueous NaOH solution, water, brine
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customPurification by silica gel chromatography