HRID1893502

反应详情

EQUATION

反应方程式

HRID 1893502 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The compound (837 mg, 2.53 mmol) obtained in step B was added to ethanol (20 ml), hydrazine monohydrate (0.31 ml, 6.4 mmol) was added, and the mixture was heated under reflux for 1 hr. The reaction mixture was cooled, and diethyl ether was added to allow precipitation of a solid. The precipitated solid was filtered, and the obtained solution was concentrated under reduced pressure to give a colorless oil. The oil was dissolved in diethyl ether, 4N hydrochloric acid-dioxane solution (1 ml) was added at room temperature and the mixture was diluted with ethyl acetate to allow precipitation of a solid. This was filtered, washed with ethyl acetate, and dried under reduced pressure to give the title compound (598 mg, yield 100%) as a colorless solid.

WORKUP

后处理

  1. additionwas added
  2. temperaturethe mixture was heated
  3. temperatureunder reflux for 1 hr
  4. temperatureThe reaction mixture was cooled
  5. customprecipitation of a solid
  6. filtrationThe precipitated solid was filtered
  7. concentrationthe obtained solution was concentrated under reduced pressure
  8. customto give a colorless oil
  9. customprecipitation of a solid
  10. filtrationThis was filtered
  11. washwashed with ethyl acetate
  12. customdried under reduced pressure