HRID619893

反应详情

EQUATION

反应方程式

HRID 619893 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a dried methanol solution (100 ml) of 3-(2'-fluoro-4'-chloro-5'-methoxycarbonyloxyphenyl)-5-isopropylidene-1,3-oxazolidine-2,4-dione (3.44 g, 10 mmol), which was synthesized by a method shown in Reference Example 12 described below, was added potassium carbonate (1.38 g, 10 mmol) and the mixture was heated at reflux for 2 hours. After the reaction was completed, the resulting mixture was quenched with an aqueous solution of ammonium chloride and extracted with ether. The ethereal extracts were dried and evaporated as small a volume as possible. The resulting residue was purified by silica gel column chromatography to give pure 3-(2'-fluoro-4'-chloro-5'-hydroxyphenyl)-5-isopropylidene-1,3-oxazolidine-2,4-dione (1.60 g).

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 2 hours
  3. customthe resulting mixture was quenched with an aqueous solution of ammonium chloride
  4. extractionextracted with ether
  5. customThe ethereal extracts were dried
  6. customevaporated as small a volume as possible
  7. customThe resulting residue was purified by silica gel column chromatography