HRID75483

反应详情

EQUATION

反应方程式

HRID 75483 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-(3-(4-(2,3-dichlorophenyl)piperazin-1-yl)propyl)isoindoline-1,3-dione (compound 36, 11.1 g, 26.5 mmol) in EtOH was added hydrazine monohydrate. The reaction mixture was stirred at room temperature for 6 hrs, then the white solid filtered off. The filtrate was concentrated under reduced pressure. The residue was diluted with CH2Cl2, and washed with water. The organic layer was dried over anhydrous MgSO4, filtered, and concentrated in vacuo. To the crude product in diethyl ether was added 2M HCl solution in diethyl ether (10 mL). The obtained product was washed with diethyl ether to provide the title compound (6.98 g, 73%) as a white solid.

WORKUP

后处理

  1. filtrationthe white solid filtered off
  2. concentrationThe filtrate was concentrated under reduced pressure
  3. additionThe residue was diluted with CH2Cl2
  4. washwashed with water
  5. dry with materialThe organic layer was dried over anhydrous MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. additionTo the crude product in diethyl ether was added 2M HCl solution in diethyl ether (10 mL)
  9. washThe obtained product was washed with diethyl ether