HRID2164620
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionwas carefully added
- customThe solvent was then removed under vacuum and water
- additionwas added to the residue
- extractionAfter basification with dilute sodium hydroxide the aqueous mixture was extracted several times with ethyl acetate
- extractionThe extract (750 mg)
- customwas dried
- customevaporated
- customto give a solid which
- customwas recrystallised from isopropanol