HRID1022769

反应详情

EQUATION

反应方程式

HRID 1022769 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-amino-3-hydroxybenzonitrile (298 mg) and potassium ethylxanthate (427 mg) in pyridine (7.4 ml) was heated under reflux for 3 hr. To the reaction mixture was added distilled water, the mixture was acidified with 1 M hydrochloric acid, and the mixture was extracted with ethyl acetate. The extract was washed with distilled water and brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel chromatography (hexane/ethyl acetate) to give the title compound (178 mg).

WORKUP

后处理

  1. temperatureunder reflux for 3 hr
  2. additionTo the reaction mixture was added
  3. distillationdistilled water
  4. extractionthe mixture was extracted with ethyl acetate
  5. washThe extract was washed with distilled water and brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customthe solvent was evaporated under reduced pressure
  8. customThe residue was purified by silica gel chromatography (hexane/ethyl acetate)