HRID434377

反应详情

EQUATION

反应方程式

HRID 434377 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 2-hydroxy-2-phenylethanamine (17.7 g) and 1-(4-carbomethoxyphenyl) propan-2-one (24.8 g) in ethanol (300 ml) was refluxed for one hour. When cooled, 10% Pd/C (1.0 g) was added and the mixture was hydrogenated on a Parr Hydrogenator at 60° and 60 psi for six hours. The mixture was filtered and the filtrate was evaporated to an oil which was taken up in methanol (75 ml). The solution was allowed to stand at 4° to give crystals (Batch 1). Ether (75 ml) was added to the mother liquors to obtain subsequent crops (Batches 2 & 3). The mother liquors were evaporated to an oil, which was crystallised from ether (Batch 4).

WORKUP

后处理

  1. temperaturewas refluxed for one hour
  2. temperatureWhen cooled
  3. customwas hydrogenated on a Parr Hydrogenator at 60°
  4. filtrationThe mixture was filtered
  5. customthe filtrate was evaporated to an oil which
  6. customto stand at 4°
  7. customto give crystals (Batch 1)
  8. customto obtain subsequent crops (Batches 2 & 3)
  9. customThe mother liquors were evaporated to an oil, which
  10. customwas crystallised from ether (Batch 4)