HRID232536

反应详情

EQUATION

反应方程式

HRID 232536 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 0.53 g (0.011 mol) of hydrazine hydrate dissolved in 25 mL ethanol was added 1.2 g (0.0089 mol) of the product from step B. The reaction mixture was refluxed for 18 hours, cooled to room temperature, concentrated under vacuum, added 100 mL H2O and extracted with ethyl acetate (3×50 mL), washed with brine (1×100 mL), dried over anhydrous magnesium sulfate, filtered and concentrated under vacuum to afford 1.0 g of a yellow solid.

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for 18 hours
  2. concentrationconcentrated under vacuum
  3. additionadded 100 mL H2O
  4. extractionextracted with ethyl acetate (3×50 mL)
  5. washwashed with brine (1×100 mL)
  6. dry with materialdried over anhydrous magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated under vacuum