HRID17657

反应详情

EQUATION

反应方程式

HRID 17657 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a stirred solution of 4′-hydroxyacetophenone (1.2 mmol) in DMF (10 mL) at rt, solid potassium carbonate (3.0 mmol) was added. 4-chlorophenethyl mesylate (1.0 mmol) was added to the reaction mixture and heated to 80° C. until completion according to General Procedure Q1, as indicated by TLC or HPLC. After cooling to rt, the reaction mixture was quenched by removing solvent in vacuuo and treating the residue with saturated sodium bicarbonate. The aqueous layer was poured into EtOAc (20 ml) and washed with H2O (2×10 ml) and brine (15 ml). The organic layer was dried over magnesium sulfate, and the solvent was removed in vacuuo to afford the desired 1-{4-[2-(4-chlorophenyl)ethoxy]phenyl}ethanone. The crude alkylated acetophenone was used for further transformation.

WORKUP

后处理

  1. temperatureAfter cooling to rt
  2. customthe reaction mixture was quenched
  3. customby removing solvent in vacuuo
  4. additiontreating the residue with saturated sodium bicarbonate
  5. additionThe aqueous layer was poured into EtOAc (20 ml)
  6. washwashed with H2O (2×10 ml) and brine (15 ml)
  7. dry with materialThe organic layer was dried over magnesium sulfate
  8. customthe solvent was removed in vacuuo