HRID11989

反应详情

EQUATION

反应方程式

HRID 11989 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

At first, 55 g of 6-bromo-1-chloro-2-naphthol (S1-2), 12.3 g of 4-pentyl-phenylboric acid (S1-3), 1.0 g of tetrakis(triphenylphosphine) palladium, 13.6 g of sodium carbonate and 100 ml of a mixed solvent of toluene/ethanol/water=3/3/1 were added to a reactor in nitrogen atmosphere and refluxed for 10 hours. The reaction solution was cooled to room temperature, added with toluene, and then washed with 1N HCl(aq) and water, dried over magnesium sulfate and distilled under a reduced pressure to remove the solvent. The residue was purified by silica gel column chromatography using toluene as an eluting solvent, and then dried under a reduced pressure to obtain 15 g of 6-(4-pentylphenyl)-1-chloro-2-naphthol (S1-4).

WORKUP

后处理

  1. temperaturerefluxed for 10 hours
  2. washwashed with 1N HCl(aq) and water
  3. dry with materialdried over magnesium sulfate
  4. distillationdistilled under a reduced pressure
  5. customto remove the solvent
  6. customThe residue was purified by silica gel column chromatography
  7. customdried under a reduced pressure