HRID2164620

反应详情

EQUATION

反应方程式

HRID 2164620 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Lithium aluminium hydride (300 mg, 7.9 mM) was added to a stirred suspension of 2-(4-carbomethoxy-2,6-dichlorophenylimino)imidazolidine (750 mg, 2.6 mM) in dry tetrahydrofuran (50 ml) with stirring. The mixture was then stirred at room temperature for several hours after which time ethyl acetate was carefully added. The solvent was then removed under vacuum and water was added to the residue. After basification with dilute sodium hydroxide the aqueous mixture was extracted several times with ethyl acetate. The extract (750 mg) was dried and evaporated to give a solid which was recrystallised from isopropanol to give a white solid (330 mg) mp 208°-210° C.

WORKUP

后处理

  1. additionwas carefully added
  2. customThe solvent was then removed under vacuum and water
  3. additionwas added to the residue
  4. extractionAfter basification with dilute sodium hydroxide the aqueous mixture was extracted several times with ethyl acetate
  5. extractionThe extract (750 mg)
  6. customwas dried
  7. customevaporated
  8. customto give a solid which
  9. customwas recrystallised from isopropanol