HRID280303
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
A mixture of 4-(4-Methylphenyl)butan-2-one (1.62 g) and 2-(3-chlorophenyl)-2-hydroxyethanamine (1.71 g) was refluxed in benzene under Dean & Stark conditions for 4 h. The solvent was removed under reduced pressure, replaced with methanol (100 ml) and sodium borohydride (2 g) added portionwise. The solvent was evaporated under reduced pressure, the residue partitioned between water and ether and the ether layer dried (MgSO4). Removal of the solvent gave an oil which was chromatographed on Kieselgel 60. Elution with 1% methanol-chloroform gave the title compound as an 11:89 mixture of diastereoisomers, mp 75-106 (hexane).
WORKUP
后处理
- customThe solvent was removed under reduced pressure
- additionadded portionwise
- customThe solvent was evaporated under reduced pressure
- customthe residue partitioned between water and ether
- dry with materialthe ether layer dried (MgSO4)
- customRemoval of the solvent
- customgave an oil which
- customwas chromatographed on Kieselgel 60
- washElution with 1% methanol-chloroform