HRID2108251

反应详情

EQUATION

反应方程式

HRID 2108251 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 31.3 g (0.115 mol) of 1-(6-bromohexyl)-2,3-dihydroxybenzene, 41 mL (0.34 mol) of benzyl bromide, 47.5 g (0.34 mol) of potassium carbonate and 4.4 mL (13.6 mmol) of tris[2-(2-methoxyethoxy)ethyl]amine (TDA-1) in 750 mL of toluene was stirred at reflux for 40 hours. The reaction mixture was washed with half-saturated brine, dried and concentrated under reduced pressure to which was purified by HPLC using 25% toluene-hexane to give 34.6 g (67% yield) of 1-(6-bromohexyl)-2,3-bis(phenylmethoxy)benzene as an oil.

WORKUP

后处理

  1. temperatureat reflux for 40 hours
  2. washThe reaction mixture was washed with half-saturated brine
  3. customdried
  4. concentrationconcentrated under reduced pressure to which
  5. customwas purified by HPLC