HRID703692

反应详情

EQUATION

反应方程式

HRID 703692 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To an acetonitrile solution (30 ml) of 3-(2'-fluoro-4'-chloro-5'-hydroxyphenyl)-5-isopropylidene-1,3-oxazolidine-2,4-dione (0.72 g, 2.5 mmol) was added sodium carbonate (0.16 g), and the mixture was heated at reflux for 1 hour. After the addition of propargyl bromide (0.36 g, 3.0 mmol), the reaction mixture was further refluxed for 1 hour. After the solution was quenched with 0.1N hdyrochloric acid, the product was extracted with chloroform. The extracts combined were dried and evaporated as small a volume as possible. The resulting pale yellow oil was purified by silica gel column chromatography to give pure 3-(2'-fluoro-4'-chloro-5'-propargyloxyphenyl)-5-isopropylidene-1,3-oxazolidine-2,4-dione. (0.53 g, 65% yield).

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 1 hour
  3. temperaturethe reaction mixture was further refluxed for 1 hour
  4. customAfter the solution was quenched with 0.1N hdyrochloric acid
  5. extractionthe product was extracted with chloroform
  6. customThe extracts combined were dried
  7. customevaporated as small a volume as possible
  8. customThe resulting pale yellow oil was purified by silica gel column chromatography