HRID638736

反应详情

EQUATION

反应方程式

HRID 638736 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 2-(4-Nitro-phenoxy)-propionic acid 47 (45 g, 213 mol) and ethylene glycol (135 ml) was passed dry HCl gas for 1½ hours. During HCl gas bubbling the temp. rose to 60° C. The crude reaction mass was poured onto cold water (600 ml). Crude 48 was extracted into chloroform, dried over Na2SO4, distilled and purified by column chromatography on silica gel using hexane as eluant to give pure 48 (28 g, 56.8%) as a syrup.

WORKUP

后处理

  1. customfor 1½ hours
  2. customDuring HCl gas bubbling the temp
  3. customrose to 60° C
  4. customThe crude reaction mass
  5. extractionCrude 48 was extracted into chloroform
  6. dry with materialdried over Na2SO4
  7. distillationdistilled
  8. custompurified by column chromatography on silica gel