HRID1357674

反应详情

EQUATION

反应方程式

HRID 1357674 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1.5 g (4 mmol) of 1-(4-hydroxyphenoxy)-2-(3-methoxyphenyl)-6-methoxynaphthalene in 40 mL of DMF was prepared. To this solution was added 920 mg (5 mmol) of 2-chloroethylpiperidine hydrochloride and 5.2 g (16 mmol) of Cs2CO3, the reaction was stirred at ambient temperature under a nitrogen atmosphere for sixteen hours. The solvents were removed by evaporation and the residue partioned between water and EtOAc. The EtOAc layer was washed with water, then brine, dried with Na2SO4, and evaporated to dryness. The residue was dissolved in 10 mL of MeOH ane 1 mL of 5N HCl was added. The solvents were removed by evaporation and the product crystallized from EtOAc. This yielded 1.8 g of the title compound as a white solid, mp 161-162° C.

WORKUP

后处理

  1. customThe solvents were removed by evaporation
  2. washThe EtOAc layer was washed with water
  3. dry with materialbrine, dried with Na2SO4
  4. customevaporated to dryness
  5. dissolutionThe residue was dissolved in 10 mL of MeOH ane 1 mL of 5N HCl
  6. additionwas added
  7. customThe solvents were removed by evaporation
  8. customthe product crystallized from EtOAc