HRID4461

反应详情

EQUATION

反应方程式

HRID 4461 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 12.0 g (42.4 mmol) 4-(4-bromo-2-fluorophenoxy)phenol, 9.5 g (42.4 mmol) methyl 4-bromo-3-methoxy-2-pentenoate, 6.45 g (46.6 mmol) potassium carbonate and 180 ml acetonitrile was heated at reflux for 16 hours. The mixture was poured into water and extracted with ether. The combined ether extracts were washed with dilute aqueous NaOH, washed with water, dried over MgSO4 and the solvent was removed by rotary evaporation. The residue was purified by HPLC eluting with 95:5 hexane:acetone, to give 10.5 g (58 percent) of the product as a clear colorless oil. Calc: C, 53.66; H, 4.27. Found: C, 53.28, H, 4.40. Structure was established on the basis of IR and NMR analysis.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 16 hours
  3. extractionextracted with ether
  4. washThe combined ether extracts were washed with dilute aqueous NaOH
  5. washwashed with water
  6. dry with materialdried over MgSO4
  7. customthe solvent was removed by rotary evaporation
  8. customThe residue was purified by HPLC
  9. washeluting with 95:5 hexane