HRID1446875

反应详情

EQUATION

反应方程式

HRID 1446875 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-[N-Methyl-N-(5-chloro-2-benzoxazolyl)amino]phenol (0.00255 mol, 0.7 g, prepared as above), ethyl 2-bromopropionate (0.00255 mol, 0.46 g) and potassium carbonate (0.00255 mol, 0.35 g) were mixed in methyl ethyl ketone (5 ml) and heated under reflux for 6 hours. The solvent was then evaporated, the residue taken into water (25 ml) and twice extracted with diethyl ether (25 ml). An oily residue was obtained which was purified by preparative thin layer chromatography on silica gel, eluent toluene/diethyl ether. Yield 0.75 g, mp 68.0°-68.6° C.; ir, and pmr spectra and analysis consistent with assigned structure.

WORKUP

后处理

  1. temperatureheated
  2. temperatureunder reflux for 6 hours
  3. customThe solvent was then evaporated
  4. extractiontwice extracted with diethyl ether (25 ml)
  5. customAn oily residue was obtained which
  6. customwas purified by preparative thin layer chromatography on silica gel, eluent toluene/diethyl ether