HRID280303

反应详情

EQUATION

反应方程式

HRID 280303 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe solvent was removed under reduced pressure
  2. additionadded portionwise
  3. customThe solvent was evaporated under reduced pressure
  4. customthe residue partitioned between water and ether
  5. dry with materialthe ether layer dried (MgSO4)
  6. customRemoval of the solvent
  7. customgave an oil which
  8. customwas chromatographed on Kieselgel 60
  9. washElution with 1% methanol-chloroform