HRID2097360

反应详情

EQUATION

反应方程式

HRID 2097360 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-[6-(4-(2-Morpholin-4-yl-ethoxy)-phenoxy)-hexyl]-phthalimide (5.46 g crude mixture from above, ≈9.67 mmol) and hydrazine hydrate (3.66 ml, 60 mmol) were dissolved in EtOH (80 mL) and stirred under reflux for 17 h. The precipitate was filtered off and washed with EtOH (1×50 mL). The filtrate was concentrated under reduced pressure, the residue was suspended in THF (20 mL) and the precipitate was filtered off, washed with THF (2×5 mL) and the filtrate was concentrated under reduced pressure to give the title compound together with some 4-(2-morpholin-4-yl-ethoxy)-phenol (≈2:1).

WORKUP

后处理

  1. temperatureunder reflux for 17 h
  2. filtrationThe precipitate was filtered off
  3. washwashed with EtOH (1×50 mL)
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. filtrationthe precipitate was filtered off
  6. washwashed with THF (2×5 mL)
  7. concentrationthe filtrate was concentrated under reduced pressure