HRID363036

反应详情

EQUATION

反应方程式

HRID 363036 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To a solution of methyl 4-hydroxybenzoate (22-1) (9.72 g, 64.36 mmol) in 100 mL of DMF was added 24.8 g (76.0 mmol) of Cs2CO3 followed by 5.0 mL (58.5 mmol) of allyl bromide. The resulting solution was then heated at 50° C. for 5 h. The solvent was distilled under reduced pressure and the residue was taken up in 200 mL of EtOAc. The organic phase was extracted with 1N NaOH (2×50 mL), water (5×50 mL) and brine (50 mL), dried (MgSO4) and concentrated to afford product 22-2 as a white solid.

WORKUP

后处理

  1. distillationThe solvent was distilled under reduced pressure
  2. extractionThe organic phase was extracted with 1N NaOH (2×50 mL), water (5×50 mL) and brine (50 mL)
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated