HRID1068806

反应详情

EQUATION

反应方程式

HRID 1068806 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 2.50 g (6.2 mmol) of 3-methyl-2-[5-(phthalimido)pentan-1-ylthio]-1,4,7b-triazacyclopent[cd]indene in 50 ml of ethanol was added 928 mg (18.5 mmol) of hydrazinemonohydrate. The mixture was heated for two hours under reflux. After cooling, the resulting precipitates were collected by filtration and washed with ethanol. The filtrate and washing were combined and concentrated to give the residue. Water was added, extracted with methylene chloride, dried over anhydrous magnesium sulfate. The solvent was distilled off to afford 1.197 g of the desired compound (70.6%, a greenish brown solid).

WORKUP

后处理

  1. additionwas added 928 mg (18.5 mmol) of hydrazinemonohydrate
  2. temperatureThe mixture was heated for two hours
  3. temperatureunder reflux
  4. temperatureAfter cooling
  5. customthe resulting precipitates
  6. filtrationwere collected by filtration
  7. washwashed with ethanol
  8. washThe filtrate and washing
  9. concentrationconcentrated
  10. customto give the residue
  11. extractionextracted with methylene chloride
  12. dry with materialdried over anhydrous magnesium sulfate
  13. distillationThe solvent was distilled off