HRID1683073

反应详情

EQUATION

反应方程式

HRID 1683073 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Combine 3-hydroxybenzoic acid (100 mmol), 2-iodopropane (500 mmol), K2CO3 (300 mmol), and 2-butanone (300 mL). Heat at reflux for 72 h. Concentrate in vacuo to obtain a residue. Add water (500 mL) and cool in an ice bath. Adjust to pH 1 by dropwise addition of concentrated HCl. Extract with dichloromethane (3×200 mL). Extract the combined organic layers with water (200 mL), dry over Na2SO4, filter, and concentrate in vacuo to obtain a residue. Purify to obtain the title compound.

WORKUP

后处理

  1. temperatureHeat
  2. temperatureat reflux for 72 h
  3. concentrationConcentrate in vacuo
  4. customto obtain a residue
  5. extractionExtract with dichloromethane (3×200 mL)
  6. extractionExtract the combined organic layers with water (200 mL)
  7. dry with materialdry over Na2SO4
  8. filtrationfilter
  9. concentrationconcentrate in vacuo
  10. customto obtain a residue
  11. customPurify